# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2233 #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Peter Andersen Department of Chemistry University of Copenhagen Universitetsparken 5 DK-2100 Copenhagen Denamrk ; _publ_contact_author_phone '045 35320113' _publ_contact_author_fax '045 35320133' _publ_contact_author_email andersen@kiku.dk _publ_requested_journal ; Dalton Transactions ; _publ_requested_coeditor_name ? _publ_contact_letter ; Here you find the crystallographic data of the publication 'Lead(IV) complexes with phosphinoyl dithioformates, R2P(O)CS2- (R=Ph,Bz). Syntheses and characterization. Crystal structures of (PPh4)[S2CP(O)Ph2]0.5H2O, [PbPh2{S2CP(O)Ph2}2] and [PbPh2Cl{S2CP(O)Ph2}]' which is submitted to the journal 'Dalton Transactions', paper ref.: Sincerely Peter Andersen ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Lead(IV) complexes with phosphinoyl dithioformates, R_2_P(O)CS_2_^-^ (R=Ph,Bz). Syntheses and characterization. Crystal structures of (PPh_4_)[S_2_CP(O)Ph_2_] 0.5H_2_O, [PbPh_2_{S_2_CP(O)Ph_2_}_2_] and [PbPh_2_Cl{S_2_CP(O)Ph_2_}] ; loop_ _publ_author_name _publ_author_address '\'Olafsson, Sigurj\'on Norberg' ; Science Institute University of Iceland Dunhaga 3 IS-107 Reykjavik Iceland ; 'Flensburg, Claus' ; Department of Chemistry University of Copenhagen Universitetsparken 5 DK-2100 Copenhagen Denmark ; 'Andersen, Peter' ; Department of Chemistry University of Copenhagen Universitetsparken 5 DK-2100 Copenhagen Denmark ; #============================================================================== data_L _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H62 O3 P4 S4' _chemical_formula_weight 1251.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.1216(14) _cell_length_b 41.242(8) _cell_length_c 9.3324(12) _cell_angle_alpha 90.00 _cell_angle_beta 117.221(11) _cell_angle_gamma 90.00 _cell_volume 3121.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 37.37 _cell_measurement_theta_max 40.28 _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 2.755 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.436 _exptl_absorpt_correction_T_max 0.854 _exptl_absorpt_process_details 'ABSORB (DeTitta, 1985)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(1) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method omega-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 5 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 seconds' _diffrn_standards_decay_% 4.9 _diffrn_reflns_number 14683 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 74.93 _reflns_number_total 12808 _reflns_number_gt 12598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS CAD4' _computing_cell_refinement 'NONIUS CAD4' _computing_data_reduction 'DREADD (Blessing, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(7) _refine_ls_number_reflns 12808 _refine_ls_number_parameters 772 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.887 _refine_ls_restrained_S_all 1.887 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1A P 1.06303(6) 0.626543(11) 0.64228(5) 0.01838(9) Uani 1 1 d . . . S1A S 1.36984(6) 0.588628(13) 0.80429(6) 0.02817(11) Uani 1 1 d . . . S2A S 1.12934(6) 0.573693(12) 0.45904(6) 0.02577(10) Uani 1 1 d . . . O1A O 1.07471(19) 0.63359(4) 0.80397(17) 0.0270(3) Uani 1 1 d . . . C1A C 1.1936(2) 0.59321(5) 0.6352(2) 0.0209(4) Uani 1 1 d . . . C11A C 1.1281(2) 0.66131(4) 0.5657(2) 0.0194(4) Uani 1 1 d . . . C12A C 1.1164(2) 0.69150(5) 0.6282(2) 0.0245(4) Uani 1 1 d . . . H12A H 1.0719 0.6930 0.7021 0.029 Uiso 1 1 calc R . . C13A C 1.1703(3) 0.71935(5) 0.5819(3) 0.0280(4) Uani 1 1 d . . . H13A H 1.1623 0.7398 0.6243 0.034 Uiso 1 1 calc R . . C14A C 1.2350(3) 0.71718(5) 0.4745(3) 0.0289(4) Uani 1 1 d . . . H14A H 1.2705 0.7363 0.4424 0.035 Uiso 1 1 calc R . . C15A C 1.2487(3) 0.68725(6) 0.4127(3) 0.0297(4) Uani 1 1 d . . . H15A H 1.2952 0.6858 0.3403 0.036 Uiso 1 1 calc R . . C16A C 1.1938(2) 0.65941(5) 0.4578(2) 0.0249(4) Uani 1 1 d . . . H16A H 1.2013 0.6390 0.4145 0.030 Uiso 1 1 calc R . . C21A C 0.8499(2) 0.61778(4) 0.5054(2) 0.0188(4) Uani 1 1 d . . . C22A C 0.7787(2) 0.62210(5) 0.3383(2) 0.0221(4) Uani 1 1 d . . . H22A H 0.8434 0.6301 0.2900 0.027 Uiso 1 1 calc R . . C23A C 0.6137(3) 0.61474(5) 0.2434(3) 0.0275(4) Uani 1 1 d . . . H23A H 0.5660 0.6175 0.1300 0.033 Uiso 1 1 calc R . . C24A C 0.5172(3) 0.60336(6) 0.3128(3) 0.0320(5) Uani 1 1 d . . . H24A H 0.4044 0.5983 0.2468 0.038 Uiso 1 1 calc R . . C25A C 0.5860(3) 0.59938(5) 0.4790(3) 0.0305(5) Uani 1 1 d . . . H25A H 0.5202 0.5919 0.5269 0.037 Uiso 1 1 calc R . . C26A C 0.7517(3) 0.60647(5) 0.5744(3) 0.0238(4) Uani 1 1 d . . . H26A H 0.7989 0.6036 0.6878 0.029 Uiso 1 1 calc R . . P2A P 0.73030(5) 0.496607(11) 0.69344(5) 0.01464(8) Uani 1 1 d . . . C31A C 0.6627(2) 0.50733(4) 0.4868(2) 0.0170(3) Uani 1 1 d . . . C32A C 0.7619(2) 0.52682(4) 0.4438(2) 0.0206(4) Uani 1 1 d . . . H32A H 0.8609 0.5359 0.5247 0.025 Uiso 1 1 calc R . . C33A C 0.7148(3) 0.53281(5) 0.2826(2) 0.0251(4) Uani 1 1 d . . . H33A H 0.7820 0.5460 0.2529 0.030 Uiso 1 1 calc R . . C34A C 0.5695(3) 0.51965(5) 0.1640(2) 0.0287(4) Uani 1 1 d . . . H34A H 0.5375 0.5239 0.0536 0.034 Uiso 1 1 calc R . . C35A C 0.4715(3) 0.50041(6) 0.2066(2) 0.0310(5) Uani 1 1 d . . . H35A H 0.3721 0.4915 0.1252 0.037 Uiso 1 1 calc R . . C36A C 0.5174(2) 0.49399(5) 0.3670(2) 0.0241(4) Uani 1 1 d . . . H36A H 0.4503 0.4806 0.3957 0.029 Uiso 1 1 calc R . . C41A C 0.8613(2) 0.46189(4) 0.7397(2) 0.0168(3) Uani 1 1 d . . . C42A C 0.9657(2) 0.45445(5) 0.9015(2) 0.0229(4) Uani 1 1 d . . . H42A H 0.9727 0.4687 0.9844 0.027 Uiso 1 1 calc R . . C43A C 1.0585(3) 0.42633(6) 0.9403(3) 0.0286(5) Uani 1 1 d . . . H43A H 1.1294 0.4212 1.0498 0.034 Uiso 1 1 calc R . . C44A C 1.0473(3) 0.40555(5) 0.8182(3) 0.0310(5) Uani 1 1 d . . . H44A H 1.1108 0.3862 0.8447 0.037 Uiso 1 1 calc R . . C45A C 0.9444(3) 0.41288(5) 0.6582(3) 0.0296(5) Uani 1 1 d . . . H45A H 0.9382 0.3986 0.5758 0.036 Uiso 1 1 calc R . . C46A C 0.8510(2) 0.44080(5) 0.6180(2) 0.0218(4) Uani 1 1 d . . . H46A H 0.7799 0.4457 0.5082 0.026 Uiso 1 1 calc R . . C51A C 0.5556(2) 0.48645(4) 0.7241(2) 0.0167(3) Uani 1 1 d . . . C52A C 0.5589(2) 0.45869(5) 0.8120(2) 0.0193(4) Uani 1 1 d . . . H52A H 0.6515 0.4446 0.8516 0.023 Uiso 1 1 calc R . . C53A C 0.4254(2) 0.45200(5) 0.8406(2) 0.0229(4) Uani 1 1 d . . . H53A H 0.4257 0.4331 0.8988 0.027 Uiso 1 1 calc R . . C54A C 0.2915(2) 0.47295(5) 0.7841(2) 0.0229(4) Uani 1 1 d . . . H54A H 0.2005 0.4683 0.8041 0.027 Uiso 1 1 calc R . . C55A C 0.2892(2) 0.50066(5) 0.6987(2) 0.0209(4) Uani 1 1 d . . . H55A H 0.1975 0.5150 0.6617 0.025 Uiso 1 1 calc R . . C56A C 0.4207(2) 0.50749(5) 0.6671(2) 0.0186(3) Uani 1 1 d . . . H56A H 0.4189 0.5263 0.6075 0.022 Uiso 1 1 calc R . . C61A C 0.8421(2) 0.52896(5) 0.8274(2) 0.0174(3) Uani 1 1 d . . . C62A C 1.0077(2) 0.53459(5) 0.8655(2) 0.0236(4) Uani 1 1 d . . . H62A H 1.0615 0.5211 0.8215 0.028 Uiso 1 1 calc R . . C63A C 1.0926(3) 0.55994(6) 0.9679(3) 0.0279(4) Uani 1 1 d . . . H63A H 1.2042 0.5639 0.9924 0.033 Uiso 1 1 calc R . . C64A C 1.0164(3) 0.57941(5) 1.0344(2) 0.0259(4) Uani 1 1 d . . . H64A H 1.0757 0.5966 1.1053 0.031 Uiso 1 1 calc R . . C65A C 0.8523(3) 0.57381(5) 0.9973(2) 0.0228(4) Uani 1 1 d . . . H65A H 0.7998 0.5872 1.0430 0.027 Uiso 1 1 calc R . . C66A C 0.7649(2) 0.54879(5) 0.8935(2) 0.0196(4) Uani 1 1 d . . . H66A H 0.6526 0.5452 0.8678 0.024 Uiso 1 1 calc R . . P1B P 0.28910(6) 0.364371(11) 0.39207(6) 0.01875(9) Uani 1 1 d . . . S1B S 0.46579(6) 0.407281(13) 0.25351(7) 0.02810(11) Uani 1 1 d . . . S2B S 0.55097(7) 0.337051(14) 0.33208(6) 0.02953(11) Uani 1 1 d . . . O1B O 0.18970(18) 0.33419(3) 0.33459(18) 0.0262(3) Uani 1 1 d . . . C1B C 0.4417(2) 0.37078(5) 0.3162(2) 0.0223(4) Uani 1 1 d . . . C11B C 0.1520(2) 0.39911(5) 0.3471(2) 0.0193(4) Uani 1 1 d . . . C12B C 0.2070(3) 0.43074(5) 0.3956(2) 0.0237(4) Uani 1 1 d . . . H12B H 0.3217 0.4348 0.4570 0.028 Uiso 1 1 calc R . . C13B C 0.0962(3) 0.45621(5) 0.3550(2) 0.0274(4) Uani 1 1 d . . . H13B H 0.1353 0.4777 0.3852 0.033 Uiso 1 1 calc R . . C14B C -0.0724(3) 0.45031(5) 0.2702(2) 0.0270(4) Uani 1 1 d . . . H14B H -0.1486 0.4678 0.2424 0.032 Uiso 1 1 calc R . . C15B C -0.1286(3) 0.41892(6) 0.2265(3) 0.0273(4) Uani 1 1 d . . . H15B H -0.2437 0.4147 0.1718 0.033 Uiso 1 1 calc R . . C16B C -0.0165(2) 0.39347(5) 0.2627(2) 0.0227(4) Uani 1 1 d . . . H16B H -0.0558 0.3721 0.2294 0.027 Uiso 1 1 calc R . . C21B C 0.4105(2) 0.36571(4) 0.6090(2) 0.0182(3) Uani 1 1 d . . . C22B C 0.5773(2) 0.37396(5) 0.6887(2) 0.0206(4) Uani 1 1 d . . . H22B H 0.6338 0.3796 0.6284 0.025 Uiso 1 1 calc R . . C23B C 0.6610(2) 0.37395(5) 0.8561(2) 0.0219(4) Uani 1 1 d . . . H23B H 0.7746 0.3795 0.9098 0.026 Uiso 1 1 calc R . . C24B C 0.5791(2) 0.36580(5) 0.9452(2) 0.0218(4) Uani 1 1 d . . . H24B H 0.6369 0.3656 1.0595 0.026 Uiso 1 1 calc R . . C25B C 0.4128(3) 0.35789(5) 0.8671(2) 0.0227(4) Uani 1 1 d . . . H25B H 0.3566 0.3524 0.9279 0.027 Uiso 1 1 calc R . . C26B C 0.3287(2) 0.35796(5) 0.6998(2) 0.0220(4) Uani 1 1 d . . . H26B H 0.2147 0.3527 0.6467 0.026 Uiso 1 1 calc R . . P2B P 0.37928(5) 0.246951(11) 0.84846(5) 0.01580(9) Uani 1 1 d . . . C31B C 0.3329(2) 0.21189(4) 0.9347(2) 0.0167(3) Uani 1 1 d . . . C32B C 0.4565(2) 0.19297(5) 1.0501(2) 0.0214(4) Uani 1 1 d . . . H32B H 0.5692 0.1978 1.0823 0.026 Uiso 1 1 calc R . . C33B C 0.4138(3) 0.16688(5) 1.1182(2) 0.0255(4) Uani 1 1 d . . . H33B H 0.4978 0.1539 1.1975 0.031 Uiso 1 1 calc R . . C34B C 0.2505(3) 0.15977(5) 1.0714(2) 0.0250(4) Uani 1 1 d . . . H34B H 0.2229 0.1421 1.1197 0.030 Uiso 1 1 calc R . . C35B C 0.1259(3) 0.17825(5) 0.9543(2) 0.0247(4) Uani 1 1 d . . . H35B H 0.0135 0.1731 0.9217 0.030 Uiso 1 1 calc R . . C36B C 0.1668(2) 0.20435(5) 0.8852(2) 0.0220(4) Uani 1 1 d . . . H36B H 0.0824 0.2170 0.8046 0.026 Uiso 1 1 calc R . . C41B C 0.3603(2) 0.23837(4) 0.6529(2) 0.0172(3) Uani 1 1 d . . . C42B C 0.3908(2) 0.26358(5) 0.5702(2) 0.0218(4) Uani 1 1 d . . . H42B H 0.4246 0.2842 0.6195 0.026 Uiso 1 1 calc R . . C43B C 0.3717(2) 0.25831(5) 0.4152(2) 0.0235(4) Uani 1 1 d . . . H43B H 0.3905 0.2754 0.3575 0.028 Uiso 1 1 calc R . . C44B C 0.3249(3) 0.22785(5) 0.3457(2) 0.0241(4) Uani 1 1 d . . . H44B H 0.3114 0.2242 0.2398 0.029 Uiso 1 1 calc R . . C45B C 0.2976(3) 0.20265(5) 0.4294(2) 0.0256(4) Uani 1 1 d . . . H45B H 0.2678 0.1818 0.3815 0.031 Uiso 1 1 calc R . . C46B C 0.3137(2) 0.20786(5) 0.5824(2) 0.0209(4) Uani 1 1 d . . . H46B H 0.2931 0.1907 0.6389 0.025 Uiso 1 1 calc R . . C51B C 0.2277(2) 0.27680(4) 0.8284(2) 0.0194(4) Uani 1 1 d . . . C52B C 0.2232(2) 0.28887(5) 0.9665(2) 0.0225(4) Uani 1 1 d . . . H52B H 0.3057 0.2826 1.0702 0.027 Uiso 1 1 calc R . . C53B C 0.0982(3) 0.31000(5) 0.9525(3) 0.0293(5) Uani 1 1 d . . . H53B H 0.0970 0.3188 1.0460 0.035 Uiso 1 1 calc R . . C54B C -0.0250(3) 0.31807(5) 0.7999(3) 0.0314(5) Uani 1 1 d . . . H54B H -0.1121 0.3320 0.7897 0.038 Uiso 1 1 calc R . . C55B C -0.0222(3) 0.30602(5) 0.6629(3) 0.0304(5) Uani 1 1 d . . . H55B H -0.1071 0.3118 0.5596 0.036 Uiso 1 1 calc R . . C56B C 0.1047(2) 0.28550(5) 0.6757(2) 0.0230(4) Uani 1 1 d . . . H56B H 0.1075 0.2775 0.5815 0.028 Uiso 1 1 calc R . . C61B C 0.5877(2) 0.25973(4) 0.9716(2) 0.0176(3) Uani 1 1 d . . . C62B C 0.7135(2) 0.24072(5) 0.9674(2) 0.0235(4) Uani 1 1 d . . . H62B H 0.6866 0.2222 0.8996 0.028 Uiso 1 1 calc R . . C63B C 0.8777(2) 0.24911(5) 1.0629(3) 0.0266(4) Uani 1 1 d . . . H63B H 0.9630 0.2362 1.0611 0.032 Uiso 1 1 calc R . . C64B C 0.9173(2) 0.27658(5) 1.1616(2) 0.0254(4) Uani 1 1 d . . . H64B H 1.0294 0.2823 1.2266 0.030 Uiso 1 1 calc R . . C65B C 0.7932(3) 0.29526(5) 1.1644(2) 0.0232(4) Uani 1 1 d . . . H65B H 0.8206 0.3139 1.2316 0.028 Uiso 1 1 calc R . . C66B C 0.6283(2) 0.28713(4) 1.0701(2) 0.0195(4) Uani 1 1 d . . . H66B H 0.5438 0.3002 1.0727 0.023 Uiso 1 1 calc R . . O3 O 1.2666(2) 0.66287(4) 1.0836(2) 0.0340(4) Uani 1 1 d . . . H1 H 1.216(4) 0.6528(8) 1.003(4) 0.041 Uiso 1 1 d . . . H2 H 1.363(4) 0.6542(8) 1.132(4) 0.041 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1A 0.0202(2) 0.0156(2) 0.0178(2) -0.00214(16) 0.00730(18) -0.00161(17) S1A 0.0201(2) 0.0238(2) 0.0286(2) 0.00007(19) 0.00077(19) 0.00039(18) S2A 0.0275(2) 0.0217(2) 0.0241(2) -0.00294(18) 0.00824(19) 0.00555(19) O1A 0.0341(8) 0.0273(8) 0.0217(7) -0.0038(6) 0.0145(6) -0.0029(6) C1A 0.0198(9) 0.0169(9) 0.0241(9) 0.0017(7) 0.0085(7) -0.0015(7) C11A 0.0163(8) 0.0154(9) 0.0212(9) -0.0019(7) 0.0041(7) -0.0014(7) C12A 0.0232(9) 0.0208(10) 0.0256(9) -0.0037(8) 0.0079(8) -0.0003(8) C13A 0.0274(10) 0.0165(10) 0.0314(11) -0.0033(8) 0.0061(9) -0.0024(8) C14A 0.0247(10) 0.0216(10) 0.0303(11) 0.0046(8) 0.0040(9) -0.0061(8) C15A 0.0273(10) 0.0333(12) 0.0274(10) 0.0030(9) 0.0116(9) -0.0041(9) C16A 0.0257(10) 0.0230(10) 0.0248(9) -0.0017(8) 0.0104(8) -0.0012(8) C21A 0.0219(9) 0.0136(9) 0.0212(9) -0.0021(7) 0.0101(8) 0.0018(7) C22A 0.0233(9) 0.0175(9) 0.0235(9) 0.0000(7) 0.0088(8) 0.0019(7) C23A 0.0253(10) 0.0205(10) 0.0270(10) -0.0018(8) 0.0036(8) 0.0040(8) C24A 0.0188(10) 0.0256(11) 0.0432(13) -0.0036(9) 0.0070(9) -0.0010(8) C25A 0.0272(11) 0.0226(10) 0.0459(13) 0.0014(9) 0.0202(10) 0.0000(8) C26A 0.0276(10) 0.0176(9) 0.0281(10) 0.0008(7) 0.0145(8) 0.0013(8) P2A 0.01441(19) 0.0136(2) 0.0169(2) 0.00084(16) 0.00803(16) 0.00020(16) C31A 0.0188(8) 0.0140(8) 0.0182(8) 0.0013(6) 0.0085(7) 0.0018(7) C32A 0.0250(9) 0.0139(8) 0.0249(9) -0.0004(7) 0.0132(8) -0.0029(7) C33A 0.0353(11) 0.0186(10) 0.0272(10) 0.0035(7) 0.0191(9) -0.0003(8) C34A 0.0376(12) 0.0281(11) 0.0204(9) 0.0058(8) 0.0132(9) 0.0023(9) C35A 0.0297(11) 0.0380(13) 0.0205(9) -0.0007(9) 0.0072(8) -0.0065(9) C36A 0.0214(9) 0.0280(10) 0.0214(9) 0.0020(8) 0.0085(7) -0.0051(8) C41A 0.0140(8) 0.0180(9) 0.0204(9) 0.0020(7) 0.0095(7) 0.0015(7) C42A 0.0212(9) 0.0270(10) 0.0237(9) 0.0060(8) 0.0132(8) 0.0010(8) C43A 0.0234(10) 0.0331(12) 0.0318(11) 0.0162(9) 0.0148(9) 0.0059(8) C44A 0.0285(10) 0.0231(10) 0.0488(13) 0.0129(9) 0.0241(10) 0.0103(8) C45A 0.0301(10) 0.0229(11) 0.0421(12) -0.0022(9) 0.0220(10) 0.0030(8) C46A 0.0211(9) 0.0197(9) 0.0260(9) 0.0000(8) 0.0120(8) 0.0014(7) C51A 0.0170(8) 0.0143(8) 0.0194(8) -0.0010(6) 0.0089(7) -0.0014(6) C52A 0.0182(8) 0.0164(9) 0.0235(9) 0.0019(7) 0.0097(7) 0.0013(7) C53A 0.0248(9) 0.0170(9) 0.0315(10) 0.0031(7) 0.0169(8) -0.0009(7) C54A 0.0191(9) 0.0230(10) 0.0298(10) -0.0007(8) 0.0141(8) -0.0036(7) C55A 0.0181(8) 0.0198(9) 0.0259(9) 0.0004(7) 0.0110(7) 0.0023(7) C56A 0.0182(8) 0.0155(8) 0.0219(9) 0.0013(7) 0.0090(7) -0.0003(7) C61A 0.0178(8) 0.0178(9) 0.0179(8) 0.0006(7) 0.0093(7) -0.0016(7) C62A 0.0182(9) 0.0286(11) 0.0239(9) -0.0040(8) 0.0096(8) -0.0020(8) C63A 0.0208(9) 0.0327(12) 0.0290(10) -0.0050(9) 0.0104(8) -0.0078(8) C64A 0.0282(10) 0.0260(11) 0.0213(9) -0.0042(7) 0.0094(8) -0.0096(8) C65A 0.0300(10) 0.0192(9) 0.0228(9) -0.0019(7) 0.0153(8) -0.0016(8) C66A 0.0225(9) 0.0173(9) 0.0227(9) 0.0004(7) 0.0136(8) -0.0001(7) P1B 0.0173(2) 0.0169(2) 0.0196(2) -0.00209(17) 0.00627(17) -0.00237(17) S1B 0.0263(2) 0.0270(3) 0.0338(3) 0.0046(2) 0.0162(2) -0.00033(19) S2B 0.0319(3) 0.0276(3) 0.0325(3) -0.0020(2) 0.0176(2) 0.0070(2) O1B 0.0255(7) 0.0187(7) 0.0310(7) -0.0068(6) 0.0098(6) -0.0067(6) C1B 0.0200(9) 0.0227(10) 0.0192(8) -0.0007(7) 0.0047(7) -0.0012(7) C11B 0.0203(9) 0.0202(10) 0.0166(8) -0.0011(7) 0.0077(7) -0.0027(7) C12B 0.0216(9) 0.0234(10) 0.0236(9) -0.0047(7) 0.0080(8) -0.0040(7) C13B 0.0308(11) 0.0220(10) 0.0246(10) -0.0038(8) 0.0086(8) -0.0001(8) C14B 0.0283(10) 0.0285(11) 0.0231(9) -0.0003(8) 0.0109(8) 0.0078(8) C15B 0.0212(9) 0.0325(11) 0.0261(10) -0.0002(8) 0.0090(8) 0.0022(8) C16B 0.0200(9) 0.0244(10) 0.0230(9) -0.0012(7) 0.0091(8) -0.0039(7) C21B 0.0198(9) 0.0131(8) 0.0210(8) 0.0002(7) 0.0088(7) -0.0014(7) C22B 0.0211(9) 0.0204(9) 0.0206(9) -0.0015(7) 0.0099(7) -0.0016(7) C23B 0.0193(9) 0.0207(10) 0.0224(9) -0.0011(7) 0.0066(7) -0.0008(7) C24B 0.0264(10) 0.0172(9) 0.0199(9) 0.0028(7) 0.0091(8) 0.0037(8) C25B 0.0266(10) 0.0179(9) 0.0276(10) 0.0066(7) 0.0158(8) 0.0023(8) C26B 0.0180(9) 0.0208(9) 0.0272(10) 0.0033(7) 0.0105(8) -0.0001(7) P2B 0.0164(2) 0.0137(2) 0.0162(2) -0.00051(16) 0.00654(17) -0.00123(16) C31B 0.0207(9) 0.0135(8) 0.0166(8) -0.0002(6) 0.0091(7) -0.0006(7) C32B 0.0198(9) 0.0199(9) 0.0230(9) -0.0002(7) 0.0085(7) 0.0010(7) C33B 0.0325(11) 0.0179(10) 0.0244(10) 0.0045(7) 0.0115(9) 0.0068(8) C34B 0.0393(11) 0.0142(9) 0.0251(9) -0.0019(7) 0.0178(9) -0.0053(8) C35B 0.0256(10) 0.0222(10) 0.0261(10) -0.0031(7) 0.0117(8) -0.0096(8) C36B 0.0184(9) 0.0221(10) 0.0210(9) 0.0010(7) 0.0052(7) -0.0025(7) C41B 0.0173(8) 0.0166(9) 0.0180(8) 0.0002(7) 0.0082(7) -0.0003(7) C42B 0.0256(10) 0.0181(9) 0.0229(9) 0.0004(7) 0.0123(8) -0.0010(7) C43B 0.0259(10) 0.0257(10) 0.0198(9) 0.0042(7) 0.0112(8) 0.0014(8) C44B 0.0265(10) 0.0288(11) 0.0185(9) -0.0027(8) 0.0116(8) 0.0019(8) C45B 0.0324(11) 0.0214(10) 0.0254(10) -0.0060(8) 0.0152(8) -0.0034(8) C46B 0.0243(9) 0.0156(9) 0.0235(9) 0.0000(7) 0.0117(8) -0.0018(7) C51B 0.0206(9) 0.0135(8) 0.0245(9) 0.0005(7) 0.0108(7) -0.0019(7) C52B 0.0235(9) 0.0214(10) 0.0253(9) -0.0006(7) 0.0136(8) -0.0033(8) C53B 0.0358(11) 0.0198(10) 0.0428(12) -0.0056(9) 0.0271(10) -0.0029(8) C54B 0.0278(10) 0.0217(10) 0.0499(13) 0.0004(9) 0.0224(10) 0.0040(8) C55B 0.0232(10) 0.0258(11) 0.0387(12) 0.0046(9) 0.0112(9) 0.0056(8) C56B 0.0216(9) 0.0213(10) 0.0238(9) -0.0003(7) 0.0083(8) 0.0016(8) C61B 0.0181(9) 0.0158(9) 0.0172(8) 0.0002(7) 0.0065(7) -0.0021(7) C62B 0.0224(9) 0.0207(10) 0.0273(10) -0.0057(7) 0.0111(8) -0.0023(7) C63B 0.0199(9) 0.0288(11) 0.0321(10) -0.0037(9) 0.0129(8) -0.0014(8) C64B 0.0193(9) 0.0271(11) 0.0269(10) 0.0004(8) 0.0081(8) -0.0058(8) C65B 0.0241(10) 0.0173(9) 0.0231(9) -0.0006(7) 0.0064(8) -0.0029(7) C66B 0.0205(9) 0.0139(9) 0.0214(9) 0.0010(7) 0.0073(7) -0.0006(7) O3 0.0311(8) 0.0323(9) 0.0286(8) -0.0087(7) 0.0049(7) 0.0040(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1A O1A 1.4918(14) . ? P1A C21A 1.809(2) . ? P1A C11A 1.818(2) . ? P1A C1A 1.839(2) . ? S1A C1A 1.670(2) . ? S2A C1A 1.678(2) . ? C11A C16A 1.390(3) . ? C11A C12A 1.399(3) . ? C12A C13A 1.393(3) . ? C12A H12A 0.9500 . ? C13A C14A 1.379(3) . ? C13A H13A 0.9500 . ? C14A C15A 1.392(3) . ? C14A H14A 0.9500 . ? C15A C16A 1.392(3) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C21A C22A 1.400(3) . ? C21A C26A 1.401(3) . ? C22A C23A 1.387(3) . ? C22A H22A 0.9500 . ? C23A C24A 1.391(3) . ? C23A H23A 0.9500 . ? C24A C25A 1.391(3) . ? C24A H24A 0.9500 . ? C25A C26A 1.389(3) . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? P2A C41A 1.7867(19) . ? P2A C31A 1.7909(18) . ? P2A C51A 1.7921(19) . ? P2A C61A 1.7934(19) . ? C31A C36A 1.397(3) . ? C31A C32A 1.399(3) . ? C32A C33A 1.384(3) . ? C32A H32A 0.9500 . ? C33A C34A 1.390(3) . ? C33A H33A 0.9500 . ? C34A C35A 1.382(3) . ? C34A H34A 0.9500 . ? C35A C36A 1.384(3) . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? C41A C46A 1.399(3) . ? C41A C42A 1.402(3) . ? C42A C43A 1.383(3) . ? C42A H42A 0.9500 . ? C43A C44A 1.393(3) . ? C43A H43A 0.9500 . ? C44A C45A 1.385(3) . ? C44A H44A 0.9500 . ? C45A C46A 1.379(3) . ? C45A H45A 0.9500 . ? C46A H46A 0.9500 . ? C51A C56A 1.397(2) . ? C51A C52A 1.401(3) . ? C52A C53A 1.389(3) . ? C52A H52A 0.9500 . ? C53A C54A 1.388(3) . ? C53A H53A 0.9500 . ? C54A C55A 1.388(3) . ? C54A H54A 0.9500 . ? C55A C56A 1.388(3) . ? C55A H55A 0.9500 . ? C56A H56A 0.9500 . ? C61A C66A 1.394(3) . ? C61A C62A 1.404(3) . ? C62A C63A 1.389(3) . ? C62A H62A 0.9500 . ? C63A C64A 1.381(3) . ? C63A H63A 0.9500 . ? C64A C65A 1.392(3) . ? C64A H64A 0.9500 . ? C65A C66A 1.390(3) . ? C65A H65A 0.9500 . ? C66A H66A 0.9500 . ? P1B O1B 1.4880(14) . ? P1B C21B 1.8105(19) . ? P1B C11B 1.820(2) . ? P1B C1B 1.847(2) . ? S1B C1B 1.666(2) . ? S2B C1B 1.678(2) . ? C11B C16B 1.389(3) . ? C11B C12B 1.397(3) . ? C12B C13B 1.385(3) . ? C12B H12B 0.9500 . ? C13B C14B 1.392(3) . ? C13B H13B 0.9500 . ? C14B C15B 1.383(3) . ? C14B H14B 0.9500 . ? C15B C16B 1.394(3) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? C21B C22B 1.396(3) . ? C21B C26B 1.398(3) . ? C22B C23B 1.390(3) . ? C22B H22B 0.9500 . ? C23B C24B 1.389(3) . ? C23B H23B 0.9500 . ? C24B C25B 1.388(3) . ? C24B H24B 0.9500 . ? C25B C26B 1.389(3) . ? C25B H25B 0.9500 . ? C26B H26B 0.9500 . ? P2B C41B 1.7877(19) . ? P2B C61B 1.7929(19) . ? P2B C51B 1.796(2) . ? P2B C31B 1.7973(19) . ? C31B C32B 1.389(3) . ? C31B C36B 1.402(3) . ? C32B C33B 1.393(3) . ? C32B H32B 0.9500 . ? C33B C34B 1.378(3) . ? C33B H33B 0.9500 . ? C34B C35B 1.390(3) . ? C34B H34B 0.9500 . ? C35B C36B 1.391(3) . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? C41B C46B 1.393(3) . ? C41B C42B 1.397(3) . ? C42B C43B 1.393(3) . ? C42B H42B 0.9500 . ? C43B C44B 1.389(3) . ? C43B H43B 0.9500 . ? C44B C45B 1.390(3) . ? C44B H44B 0.9500 . ? C45B C46B 1.383(3) . ? C45B H45B 0.9500 . ? C46B H46B 0.9500 . ? C51B C56B 1.399(3) . ? C51B C52B 1.400(3) . ? C52B C53B 1.393(3) . ? C52B H52B 0.9500 . ? C53B C54B 1.392(3) . ? C53B H53B 0.9500 . ? C54B C55B 1.382(3) . ? C54B H54B 0.9500 . ? C55B C56B 1.394(3) . ? C55B H55B 0.9500 . ? C56B H56B 0.9500 . ? C61B C66B 1.395(3) . ? C61B C62B 1.405(3) . ? C62B C63B 1.391(3) . ? C62B H62B 0.9500 . ? C63B C64B 1.399(3) . ? C63B H63B 0.9500 . ? C64B C65B 1.379(3) . ? C64B H64B 0.9500 . ? C65B C66B 1.392(3) . ? C65B H65B 0.9500 . ? C66B H66B 0.9500 . ? O3 H1 0.80(3) . ? O3 H2 0.86(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A P1A C21A 108.04(9) . . ? O1A P1A C11A 111.04(9) . . ? C21A P1A C11A 108.57(9) . . ? O1A P1A C1A 115.70(9) . . ? C21A P1A C1A 109.27(9) . . ? C11A P1A C1A 104.02(9) . . ? S1A C1A S2A 128.70(13) . . ? S1A C1A P1A 114.22(11) . . ? S2A C1A P1A 116.88(11) . . ? C16A C11A C12A 119.47(19) . . ? C16A C11A P1A 124.53(15) . . ? C12A C11A P1A 115.92(15) . . ? C13A C12A C11A 120.0(2) . . ? C13A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? C14A C13A C12A 120.0(2) . . ? C14A C13A H13A 120.0 . . ? C12A C13A H13A 120.0 . . ? C13A C14A C15A 120.5(2) . . ? C13A C14A H14A 119.7 . . ? C15A C14A H14A 119.7 . . ? C14A C15A C16A 119.5(2) . . ? C14A C15A H15A 120.2 . . ? C16A C15A H15A 120.2 . . ? C11A C16A C15A 120.4(2) . . ? C11A C16A H16A 119.8 . . ? C15A C16A H16A 119.8 . . ? C22A C21A C26A 119.11(18) . . ? C22A C21A P1A 124.22(15) . . ? C26A C21A P1A 116.67(14) . . ? C23A C22A C21A 119.88(19) . . ? C23A C22A H22A 120.1 . . ? C21A C22A H22A 120.1 . . ? C22A C23A C24A 120.6(2) . . ? C22A C23A H23A 119.7 . . ? C24A C23A H23A 119.7 . . ? C25A C24A C23A 120.0(2) . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C26A C25A C24A 119.6(2) . . ? C26A C25A H25A 120.2 . . ? C24A C25A H25A 120.2 . . ? C25A C26A C21A 120.8(2) . . ? C25A C26A H26A 119.6 . . ? C21A C26A H26A 119.6 . . ? C41A P2A C31A 108.71(8) . . ? C41A P2A C51A 108.63(8) . . ? C31A P2A C51A 109.63(9) . . ? C41A P2A C61A 108.89(9) . . ? C31A P2A C61A 111.88(8) . . ? C51A P2A C61A 109.04(8) . . ? C36A C31A C32A 119.85(17) . . ? C36A C31A P2A 119.84(14) . . ? C32A C31A P2A 120.09(14) . . ? C33A C32A C31A 119.60(18) . . ? C33A C32A H32A 120.2 . . ? C31A C32A H32A 120.2 . . ? C32A C33A C34A 120.27(19) . . ? C32A C33A H33A 119.9 . . ? C34A C33A H33A 119.9 . . ? C35A C34A C33A 120.11(19) . . ? C35A C34A H34A 119.9 . . ? C33A C34A H34A 119.9 . . ? C34A C35A C36A 120.4(2) . . ? C34A C35A H35A 119.8 . . ? C36A C35A H35A 119.8 . . ? C35A C36A C31A 119.80(19) . . ? C35A C36A H36A 120.1 . . ? C31A C36A H36A 120.1 . . ? C46A C41A C42A 119.90(18) . . ? C46A C41A P2A 120.87(14) . . ? C42A C41A P2A 119.01(14) . . ? C43A C42A C41A 119.9(2) . . ? C43A C42A H42A 120.1 . . ? C41A C42A H42A 120.1 . . ? C42A C43A C44A 119.7(2) . . ? C42A C43A H43A 120.2 . . ? C44A C43A H43A 120.2 . . ? C45A C44A C43A 120.5(2) . . ? C45A C44A H44A 119.7 . . ? C43A C44A H44A 119.7 . . ? C46A C45A C44A 120.4(2) . . ? C46A C45A H45A 119.8 . . ? C44A C45A H45A 119.8 . . ? C45A C46A C41A 119.65(19) . . ? C45A C46A H46A 120.2 . . ? C41A C46A H46A 120.2 . . ? C56A C51A C52A 120.63(17) . . ? C56A C51A P2A 119.15(14) . . ? C52A C51A P2A 120.12(14) . . ? C53A C52A C51A 119.28(17) . . ? C53A C52A H52A 120.4 . . ? C51A C52A H52A 120.4 . . ? C54A C53A C52A 120.02(18) . . ? C54A C53A H53A 120.0 . . ? C52A C53A H53A 120.0 . . ? C55A C54A C53A 120.63(18) . . ? C55A C54A H54A 119.7 . . ? C53A C54A H54A 119.7 . . ? C54A C55A C56A 120.12(18) . . ? C54A C55A H55A 119.9 . . ? C56A C55A H55A 119.9 . . ? C55A C56A C51A 119.30(17) . . ? C55A C56A H56A 120.3 . . ? C51A C56A H56A 120.3 . . ? C66A C61A C62A 119.57(18) . . ? C66A C61A P2A 120.25(14) . . ? C62A C61A P2A 120.17(15) . . ? C63A C62A C61A 119.72(19) . . ? C63A C62A H62A 120.1 . . ? C61A C62A H62A 120.1 . . ? C64A C63A C62A 120.66(19) . . ? C64A C63A H63A 119.7 . . ? C62A C63A H63A 119.7 . . ? C63A C64A C65A 119.74(19) . . ? C63A C64A H64A 120.1 . . ? C65A C64A H64A 120.1 . . ? C66A C65A C64A 120.39(18) . . ? C66A C65A H65A 119.8 . . ? C64A C65A H65A 119.8 . . ? C65A C66A C61A 119.91(18) . . ? C65A C66A H66A 120.0 . . ? C61A C66A H66A 120.0 . . ? O1B P1B C21B 112.88(9) . . ? O1B P1B C11B 109.52(9) . . ? C21B P1B C11B 103.78(8) . . ? O1B P1B C1B 115.05(9) . . ? C21B P1B C1B 103.98(9) . . ? C11B P1B C1B 110.96(9) . . ? S1B C1B S2B 127.71(13) . . ? S1B C1B P1B 120.51(12) . . ? S2B C1B P1B 111.66(11) . . ? C16B C11B C12B 118.70(18) . . ? C16B C11B P1B 117.68(15) . . ? C12B C11B P1B 123.60(15) . . ? C13B C12B C11B 120.71(19) . . ? C13B C12B H12B 119.6 . . ? C11B C12B H12B 119.6 . . ? C12B C13B C14B 120.1(2) . . ? C12B C13B H13B 120.0 . . ? C14B C13B H13B 120.0 . . ? C15B C14B C13B 119.67(19) . . ? C15B C14B H14B 120.2 . . ? C13B C14B H14B 120.2 . . ? C14B C15B C16B 120.09(19) . . ? C14B C15B H15B 120.0 . . ? C16B C15B H15B 120.0 . . ? C11B C16B C15B 120.66(19) . . ? C11B C16B H16B 119.7 . . ? C15B C16B H16B 119.7 . . ? C22B C21B C26B 119.12(17) . . ? C22B C21B P1B 124.29(14) . . ? C26B C21B P1B 116.59(14) . . ? C23B C22B C21B 120.21(18) . . ? C23B C22B H22B 119.9 . . ? C21B C22B H22B 119.9 . . ? C24B C23B C22B 120.22(19) . . ? C24B C23B H23B 119.9 . . ? C22B C23B H23B 119.9 . . ? C25B C24B C23B 120.02(18) . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C24B C25B C26B 119.90(18) . . ? C24B C25B H25B 120.1 . . ? C26B C25B H25B 120.1 . . ? C25B C26B C21B 120.52(18) . . ? C25B C26B H26B 119.7 . . ? C21B C26B H26B 119.7 . . ? C41B P2B C61B 106.97(9) . . ? C41B P2B C51B 108.58(9) . . ? C61B P2B C51B 113.92(9) . . ? C41B P2B C31B 111.42(8) . . ? C61B P2B C31B 110.32(9) . . ? C51B P2B C31B 105.70(9) . . ? C32B C31B C36B 120.19(17) . . ? C32B C31B P2B 121.68(14) . . ? C36B C31B P2B 118.11(14) . . ? C31B C32B C33B 119.35(18) . . ? C31B C32B H32B 120.3 . . ? C33B C32B H32B 120.3 . . ? C34B C33B C32B 120.48(18) . . ? C34B C33B H33B 119.8 . . ? C32B C33B H33B 119.8 . . ? C33B C34B C35B 120.62(19) . . ? C33B C34B H34B 119.7 . . ? C35B C34B H34B 119.7 . . ? C34B C35B C36B 119.49(19) . . ? C34B C35B H35B 120.3 . . ? C36B C35B H35B 120.3 . . ? C35B C36B C31B 119.86(18) . . ? C35B C36B H36B 120.1 . . ? C31B C36B H36B 120.1 . . ? C46B C41B C42B 120.40(17) . . ? C46B C41B P2B 121.82(14) . . ? C42B C41B P2B 117.77(14) . . ? C43B C42B C41B 119.72(18) . . ? C43B C42B H42B 120.1 . . ? C41B C42B H42B 120.1 . . ? C44B C43B C42B 119.50(18) . . ? C44B C43B H43B 120.3 . . ? C42B C43B H43B 120.3 . . ? C43B C44B C45B 120.63(18) . . ? C43B C44B H44B 119.7 . . ? C45B C44B H44B 119.7 . . ? C46B C45B C44B 120.18(19) . . ? C46B C45B H45B 119.9 . . ? C44B C45B H45B 119.9 . . ? C45B C46B C41B 119.55(18) . . ? C45B C46B H46B 120.2 . . ? C41B C46B H46B 120.2 . . ? C56B C51B C52B 119.97(18) . . ? C56B C51B P2B 120.17(15) . . ? C52B C51B P2B 119.55(15) . . ? C53B C52B C51B 120.23(19) . . ? C53B C52B H52B 119.9 . . ? C51B C52B H52B 119.9 . . ? C54B C53B C52B 119.2(2) . . ? C54B C53B H53B 120.4 . . ? C52B C53B H53B 120.4 . . ? C55B C54B C53B 120.8(2) . . ? C55B C54B H54B 119.6 . . ? C53B C54B H54B 119.6 . . ? C54B C55B C56B 120.3(2) . . ? C54B C55B H55B 119.8 . . ? C56B C55B H55B 119.8 . . ? C55B C56B C51B 119.36(19) . . ? C55B C56B H56B 120.3 . . ? C51B C56B H56B 120.3 . . ? C66B C61B C62B 119.75(17) . . ? C66B C61B P2B 122.98(14) . . ? C62B C61B P2B 117.27(14) . . ? C63B C62B C61B 119.78(18) . . ? C63B C62B H62B 120.1 . . ? C61B C62B H62B 120.1 . . ? C62B C63B C64B 120.09(19) . . ? C62B C63B H63B 120.0 . . ? C64B C63B H63B 120.0 . . ? C65B C64B C63B 119.85(19) . . ? C65B C64B H64B 120.1 . . ? C63B C64B H64B 120.1 . . ? C64B C65B C66B 120.80(19) . . ? C64B C65B H65B 119.6 . . ? C66B C65B H65B 119.6 . . ? C65B C66B C61B 119.73(18) . . ? C65B C66B H66B 120.1 . . ? C61B C66B H66B 120.1 . . ? H1 O3 H2 107(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A P1A C1A S1A -31.08(14) . . . . ? C21A P1A C1A S1A -153.24(10) . . . . ? C11A P1A C1A S1A 90.98(12) . . . . ? O1A P1A C1A S2A 153.65(10) . . . . ? C21A P1A C1A S2A 31.49(14) . . . . ? C11A P1A C1A S2A -84.29(12) . . . . ? O1A P1A C11A C16A 153.05(17) . . . . ? C21A P1A C11A C16A -88.32(18) . . . . ? C1A P1A C11A C16A 27.95(19) . . . . ? O1A P1A C11A C12A -23.85(18) . . . . ? C21A P1A C11A C12A 94.78(16) . . . . ? C1A P1A C11A C12A -148.95(15) . . . . ? C16A C11A C12A C13A 0.1(3) . . . . ? P1A C11A C12A C13A 177.19(16) . . . . ? C11A C12A C13A C14A 0.0(3) . . . . ? C12A C13A C14A C15A -0.6(3) . . . . ? C13A C14A C15A C16A 1.1(3) . . . . ? C12A C11A C16A C15A 0.4(3) . . . . ? P1A C11A C16A C15A -176.39(16) . . . . ? C14A C15A C16A C11A -1.0(3) . . . . ? O1A P1A C21A C22A 154.60(16) . . . . ? C11A P1A C21A C22A 34.09(19) . . . . ? C1A P1A C21A C22A -78.74(18) . . . . ? O1A P1A C21A C26A -24.34(17) . . . . ? C11A P1A C21A C26A -144.85(15) . . . . ? C1A P1A C21A C26A 102.32(15) . . . . ? C26A C21A C22A C23A -0.9(3) . . . . ? P1A C21A C22A C23A -179.84(15) . . . . ? C21A C22A C23A C24A 0.6(3) . . . . ? C22A C23A C24A C25A 0.2(3) . . . . ? C23A C24A C25A C26A -0.8(3) . . . . ? C24A C25A C26A C21A 0.4(3) . . . . ? C22A C21A C26A C25A 0.4(3) . . . . ? P1A C21A C26A C25A 179.41(16) . . . . ? C41A P2A C31A C36A 90.19(17) . . . . ? C51A P2A C31A C36A -28.42(18) . . . . ? C61A P2A C31A C36A -149.51(16) . . . . ? C41A P2A C31A C32A -84.40(16) . . . . ? C51A P2A C31A C32A 156.99(15) . . . . ? C61A P2A C31A C32A 35.89(17) . . . . ? C36A C31A C32A C33A 0.2(3) . . . . ? P2A C31A C32A C33A 174.80(15) . . . . ? C31A C32A C33A C34A 0.2(3) . . . . ? C32A C33A C34A C35A -0.2(3) . . . . ? C33A C34A C35A C36A -0.2(4) . . . . ? C34A C35A C36A C31A 0.7(3) . . . . ? C32A C31A C36A C35A -0.7(3) . . . . ? P2A C31A C36A C35A -175.27(17) . . . . ? C31A P2A C41A C46A -23.21(18) . . . . ? C51A P2A C41A C46A 96.03(16) . . . . ? C61A P2A C41A C46A -145.33(15) . . . . ? C31A P2A C41A C42A 162.07(14) . . . . ? C51A P2A C41A C42A -78.69(16) . . . . ? C61A P2A C41A C42A 39.94(17) . . . . ? C46A C41A C42A C43A 0.2(3) . . . . ? P2A C41A C42A C43A 174.95(15) . . . . ? C41A C42A C43A C44A -0.1(3) . . . . ? C42A C43A C44A C45A 0.1(3) . . . . ? C43A C44A C45A C46A -0.3(3) . . . . ? C44A C45A C46A C41A 0.4(3) . . . . ? C42A C41A C46A C45A -0.4(3) . . . . ? P2A C41A C46A C45A -175.04(16) . . . . ? C41A P2A C51A C56A -167.98(14) . . . . ? C31A P2A C51A C56A -49.33(17) . . . . ? C61A P2A C51A C56A 73.47(17) . . . . ? C41A P2A C51A C52A 15.58(18) . . . . ? C31A P2A C51A C52A 134.24(15) . . . . ? C61A P2A C51A C52A -102.96(16) . . . . ? C56A C51A C52A C53A 0.8(3) . . . . ? P2A C51A C52A C53A 177.14(15) . . . . ? C51A C52A C53A C54A -0.8(3) . . . . ? C52A C53A C54A C55A 0.1(3) . . . . ? C53A C54A C55A C56A 0.8(3) . . . . ? C54A C55A C56A C51A -0.8(3) . . . . ? C52A C51A C56A C55A 0.1(3) . . . . ? P2A C51A C56A C55A -176.34(14) . . . . ? C41A P2A C61A C66A -139.07(15) . . . . ? C31A P2A C61A C66A 100.74(16) . . . . ? C51A P2A C61A C66A -20.70(18) . . . . ? C41A P2A C61A C62A 41.27(18) . . . . ? C31A P2A C61A C62A -78.92(17) . . . . ? C51A P2A C61A C62A 159.64(15) . . . . ? C66A C61A C62A C63A -0.4(3) . . . . ? P2A C61A C62A C63A 179.26(16) . . . . ? C61A C62A C63A C64A 0.9(3) . . . . ? C62A C63A C64A C65A -0.7(3) . . . . ? C63A C64A C65A C66A -0.1(3) . . . . ? C64A C65A C66A C61A 0.6(3) . . . . ? C62A C61A C66A C65A -0.4(3) . . . . ? P2A C61A C66A C65A 179.98(15) . . . . ? O1B P1B C1B S1B 137.00(12) . . . . ? C21B P1B C1B S1B -99.04(13) . . . . ? C11B P1B C1B S1B 11.96(15) . . . . ? O1B P1B C1B S2B -46.59(13) . . . . ? C21B P1B C1B S2B 77.37(12) . . . . ? C11B P1B C1B S2B -171.63(10) . . . . ? O1B P1B C11B C16B -3.17(17) . . . . ? C21B P1B C11B C16B -123.95(15) . . . . ? C1B P1B C11B C16B 124.93(15) . . . . ? O1B P1B C11B C12B 175.43(16) . . . . ? C21B P1B C11B C12B 54.65(18) . . . . ? C1B P1B C11B C12B -56.47(19) . . . . ? C16B C11B C12B C13B -2.5(3) . . . . ? P1B C11B C12B C13B 178.95(16) . . . . ? C11B C12B C13B C14B 2.4(3) . . . . ? C12B C13B C14B C15B 0.0(3) . . . . ? C13B C14B C15B C16B -2.1(3) . . . . ? C12B C11B C16B C15B 0.3(3) . . . . ? P1B C11B C16B C15B 178.97(16) . . . . ? C14B C15B C16B C11B 2.0(3) . . . . ? O1B P1B C21B C22B 132.34(16) . . . . ? C11B P1B C21B C22B -109.17(17) . . . . ? C1B P1B C21B C22B 6.98(19) . . . . ? O1B P1B C21B C26B -47.83(17) . . . . ? C11B P1B C21B C26B 70.66(16) . . . . ? C1B P1B C21B C26B -173.19(15) . . . . ? C26B C21B C22B C23B 1.0(3) . . . . ? P1B C21B C22B C23B -179.22(15) . . . . ? C21B C22B C23B C24B -0.2(3) . . . . ? C22B C23B C24B C25B -0.5(3) . . . . ? C23B C24B C25B C26B 0.4(3) . . . . ? C24B C25B C26B C21B 0.5(3) . . . . ? C22B C21B C26B C25B -1.1(3) . . . . ? P1B C21B C26B C25B 179.05(15) . . . . ? C41B P2B C31B C32B 101.19(17) . . . . ? C61B P2B C31B C32B -17.46(18) . . . . ? C51B P2B C31B C32B -141.05(16) . . . . ? C41B P2B C31B C36B -80.32(16) . . . . ? C61B P2B C31B C36B 161.03(15) . . . . ? C51B P2B C31B C36B 37.45(17) . . . . ? C36B C31B C32B C33B -1.3(3) . . . . ? P2B C31B C32B C33B 177.21(15) . . . . ? C31B C32B C33B C34B 0.2(3) . . . . ? C32B C33B C34B C35B 0.7(3) . . . . ? C33B C34B C35B C36B -0.7(3) . . . . ? C34B C35B C36B C31B -0.4(3) . . . . ? C32B C31B C36B C35B 1.3(3) . . . . ? P2B C31B C36B C35B -177.18(15) . . . . ? C61B P2B C41B C46B 121.05(16) . . . . ? C51B P2B C41B C46B -115.60(16) . . . . ? C31B P2B C41B C46B 0.41(19) . . . . ? C61B P2B C41B C42B -60.11(17) . . . . ? C51B P2B C41B C42B 63.24(17) . . . . ? C31B P2B C41B C42B 179.25(14) . . . . ? C46B C41B C42B C43B 1.2(3) . . . . ? P2B C41B C42B C43B -177.69(15) . . . . ? C41B C42B C43B C44B -1.0(3) . . . . ? C42B C43B C44B C45B -0.2(3) . . . . ? C43B C44B C45B C46B 1.3(3) . . . . ? C44B C45B C46B C41B -1.1(3) . . . . ? C42B C41B C46B C45B -0.1(3) . . . . ? P2B C41B C46B C45B 178.72(15) . . . . ? C41B P2B C51B C56B 9.74(18) . . . . ? C61B P2B C51B C56B 128.81(16) . . . . ? C31B P2B C51B C56B -109.91(16) . . . . ? C41B P2B C51B C52B -176.72(15) . . . . ? C61B P2B C51B C52B -57.65(17) . . . . ? C31B P2B C51B C52B 63.63(17) . . . . ? C56B C51B C52B C53B -1.2(3) . . . . ? P2B C51B C52B C53B -174.72(15) . . . . ? C51B C52B C53B C54B 2.2(3) . . . . ? C52B C53B C54B C55B -1.6(3) . . . . ? C53B C54B C55B C56B 0.0(3) . . . . ? C54B C55B C56B C51B 1.0(3) . . . . ? C52B C51B C56B C55B -0.4(3) . . . . ? P2B C51B C56B C55B 173.08(16) . . . . ? C41B P2B C61B C66B 132.90(16) . . . . ? C51B P2B C61B C66B 12.91(19) . . . . ? C31B P2B C61B C66B -105.76(17) . . . . ? C41B P2B C61B C62B -47.58(17) . . . . ? C51B P2B C61B C62B -167.57(14) . . . . ? C31B P2B C61B C62B 73.76(17) . . . . ? C66B C61B C62B C63B 0.8(3) . . . . ? P2B C61B C62B C63B -178.73(16) . . . . ? C61B C62B C63B C64B -0.6(3) . . . . ? C62B C63B C64B C65B 0.2(3) . . . . ? C63B C64B C65B C66B 0.0(3) . . . . ? C64B C65B C66B C61B 0.2(3) . . . . ? C62B C61B C66B C65B -0.6(3) . . . . ? P2B C61B C66B C65B 178.94(15) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 74.93 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.212 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.043 ### END data_1A _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H30 O2 P2 Pb S4' _chemical_formula_weight 915.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.403(3) _cell_length_b 17.634(5) _cell_length_c 14.420(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.03(2) _cell_angle_gamma 90.00 _cell_volume 3662.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.25 _cell_measurement_theta_max 21.73 _exptl_crystal_description stick _exptl_crystal_colour violet _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 4.955 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.368 _exptl_absorpt_correction_T_max 0.550 _exptl_absorpt_process_details 'ABSORB (DeTitta, 1985)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method omega-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 5 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 seconds' _diffrn_standards_decay_% 7.9 _diffrn_reflns_number 15143 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 29.97 _reflns_number_total 10630 _reflns_number_gt 8528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS CAD4' _computing_cell_refinement 'NONIUS CAD4' _computing_data_reduction 'DREADD (Blessing, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10630 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_restrained_S_all 1.220 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb Pb 0.627697(10) 0.085929(8) 0.276471(10) 0.01966(5) Uani 1 1 d . . . S1 S 0.73374(7) 0.17933(6) 0.17085(8) 0.0263(2) Uani 1 1 d . . . S2 S 0.92945(8) 0.17014(8) 0.10395(8) 0.0328(3) Uani 1 1 d . . . S3 S 0.50729(7) 0.17881(6) 0.18818(7) 0.0261(2) Uani 1 1 d . . . S4 S 0.30930(8) 0.21634(8) 0.21930(10) 0.0382(3) Uani 1 1 d . . . P1 P 0.87288(7) 0.07888(6) 0.26873(7) 0.0217(2) Uani 1 1 d . . . P2 P 0.38286(7) 0.06813(6) 0.28947(7) 0.0215(2) Uani 1 1 d . . . O1 O 0.7870(2) 0.05382(17) 0.31947(19) 0.0245(6) Uani 1 1 d . . . O2 O 0.47410(19) 0.03266(16) 0.31609(19) 0.0225(6) Uani 1 1 d . . . C1 C 0.8446(3) 0.1451(2) 0.1742(3) 0.0218(8) Uani 1 1 d . . . C2 C 0.3999(3) 0.1602(3) 0.2324(3) 0.0250(8) Uani 1 1 d . . . C11 C 0.6249(3) 0.1374(2) 0.4143(3) 0.0206(8) Uani 1 1 d . . . C12 C 0.6688(3) 0.2059(2) 0.4283(3) 0.0294(9) Uani 1 1 d . . . H12 H 0.6991 0.2310 0.3785 0.035 Uiso 1 1 calc R . . C13 C 0.6681(3) 0.2377(3) 0.5165(3) 0.0328(10) Uani 1 1 d . . . H13 H 0.6974 0.2852 0.5271 0.039 Uiso 1 1 calc R . . C14 C 0.6247(3) 0.2002(3) 0.5889(3) 0.0316(10) Uani 1 1 d . . . H14 H 0.6247 0.2218 0.6492 0.038 Uiso 1 1 calc R . . C15 C 0.5814(3) 0.1315(3) 0.5734(3) 0.0330(10) Uani 1 1 d . . . H15 H 0.5516 0.1060 0.6232 0.040 Uiso 1 1 calc R . . C16 C 0.5814(3) 0.0994(3) 0.4858(3) 0.0310(10) Uani 1 1 d . . . H16 H 0.5518 0.0521 0.4751 0.037 Uiso 1 1 calc R . . C21 C 0.6302(3) -0.0123(2) 0.1867(3) 0.0247(8) Uani 1 1 d . . . C22 C 0.6406(4) -0.0841(3) 0.2226(4) 0.0433(13) Uani 1 1 d . . . H22 H 0.6489 -0.0908 0.2874 0.052 Uiso 1 1 calc R . . C23 C 0.6389(4) -0.1465(3) 0.1643(5) 0.0526(15) Uani 1 1 d . . . H23 H 0.6471 -0.1961 0.1888 0.063 Uiso 1 1 calc R . . C24 C 0.6254(4) -0.1364(3) 0.0701(4) 0.0510(15) Uani 1 1 d . . . H24 H 0.6252 -0.1791 0.0300 0.061 Uiso 1 1 calc R . . C25 C 0.6124(5) -0.0657(3) 0.0348(4) 0.0521(15) Uani 1 1 d . . . H25 H 0.6016 -0.0594 -0.0298 0.062 Uiso 1 1 calc R . . C26 C 0.6148(4) -0.0025(3) 0.0929(3) 0.0400(12) Uani 1 1 d . . . H26 H 0.6060 0.0469 0.0681 0.048 Uiso 1 1 calc R . . C31 C 0.9319(3) -0.0011(2) 0.2203(3) 0.0276(9) Uani 1 1 d . . . C32 C 0.9022(4) -0.0303(3) 0.1350(4) 0.0410(12) Uani 1 1 d . . . H32 H 0.8589 -0.0032 0.0980 0.049 Uiso 1 1 calc R . . C33 C 0.9374(5) -0.0998(3) 0.1056(5) 0.0540(16) Uani 1 1 d . . . H33 H 0.9179 -0.1204 0.0479 0.065 Uiso 1 1 calc R . . C34 C 0.9999(5) -0.1387(3) 0.1592(5) 0.0546(17) Uani 1 1 d . . . H34 H 1.0228 -0.1864 0.1386 0.066 Uiso 1 1 calc R . . C35 C 1.0297(4) -0.1099(3) 0.2416(4) 0.0502(15) Uani 1 1 d . . . H35 H 1.0741 -0.1370 0.2773 0.060 Uiso 1 1 calc R . . C36 C 0.9954(4) -0.0413(3) 0.2736(3) 0.0362(11) Uani 1 1 d . . . H36 H 1.0152 -0.0219 0.3318 0.043 Uiso 1 1 calc R . . C41 C 0.9481(3) 0.1292(2) 0.3453(3) 0.0217(8) Uani 1 1 d . . . C42 C 1.0372(3) 0.1538(3) 0.3209(3) 0.0284(9) Uani 1 1 d . . . H42 H 1.0608 0.1430 0.2609 0.034 Uiso 1 1 calc R . . C43 C 1.0915(3) 0.1937(3) 0.3836(3) 0.0333(10) Uani 1 1 d . . . H43 H 1.1521 0.2101 0.3672 0.040 Uiso 1 1 calc R . . C44 C 1.0551(3) 0.2095(3) 0.4721(3) 0.0350(11) Uani 1 1 d . . . H44 H 1.0916 0.2370 0.5154 0.042 Uiso 1 1 calc R . . C45 C 0.9679(3) 0.1858(3) 0.4968(3) 0.0314(10) Uani 1 1 d . . . H45 H 0.9448 0.1968 0.5570 0.038 Uiso 1 1 calc R . . C46 C 0.9131(3) 0.1458(2) 0.4342(3) 0.0248(8) Uani 1 1 d . . . H46 H 0.8526 0.1297 0.4513 0.030 Uiso 1 1 calc R . . C51 C 0.3220(3) 0.0098(3) 0.2080(3) 0.0256(9) Uani 1 1 d . . . C52 C 0.3666(3) -0.0550(3) 0.1759(3) 0.0319(10) Uani 1 1 d . . . H52 H 0.4272 -0.0672 0.1972 0.038 Uiso 1 1 calc R . . C53 C 0.3216(4) -0.1019(3) 0.1122(4) 0.0424(13) Uani 1 1 d . . . H53 H 0.3515 -0.1466 0.0904 0.051 Uiso 1 1 calc R . . C54 C 0.2351(4) -0.0840(3) 0.0810(4) 0.0474(14) Uani 1 1 d . . . H54 H 0.2052 -0.1164 0.0376 0.057 Uiso 1 1 calc R . . C55 C 0.1903(4) -0.0199(4) 0.1115(4) 0.0457(14) Uani 1 1 d . . . H55 H 0.1298 -0.0083 0.0894 0.055 Uiso 1 1 calc R . . C56 C 0.2338(3) 0.0280(3) 0.1748(3) 0.0345(11) Uani 1 1 d . . . H56 H 0.2036 0.0728 0.1953 0.041 Uiso 1 1 calc R . . C61 C 0.3115(3) 0.0837(2) 0.3889(3) 0.0232(8) Uani 1 1 d . . . C62 C 0.3370(3) 0.1403(3) 0.4518(3) 0.0280(9) Uani 1 1 d . . . H62 H 0.3863 0.1741 0.4373 0.034 Uiso 1 1 calc R . . C63 C 0.2901(3) 0.1471(3) 0.5356(3) 0.0318(10) Uani 1 1 d . . . H63 H 0.3073 0.1856 0.5784 0.038 Uiso 1 1 calc R . . C64 C 0.2188(4) 0.0981(3) 0.5569(3) 0.0348(11) Uani 1 1 d . . . H64 H 0.1873 0.1028 0.6145 0.042 Uiso 1 1 calc R . . C65 C 0.1927(3) 0.0421(3) 0.4951(3) 0.0319(10) Uani 1 1 d . . . H65 H 0.1430 0.0089 0.5101 0.038 Uiso 1 1 calc R . . C66 C 0.2387(3) 0.0343(2) 0.4113(3) 0.0274(9) Uani 1 1 d . . . H66 H 0.2210 -0.0045 0.3691 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb 0.02162(7) 0.01875(7) 0.01860(7) -0.00007(6) 0.00149(5) -0.00235(6) S1 0.0243(5) 0.0264(5) 0.0283(5) 0.0088(4) 0.0024(4) -0.0025(4) S2 0.0272(5) 0.0437(7) 0.0273(5) 0.0055(5) 0.0059(4) -0.0047(5) S3 0.0257(5) 0.0265(5) 0.0261(5) 0.0085(4) 0.0040(4) -0.0001(4) S4 0.0258(5) 0.0391(7) 0.0497(7) 0.0170(6) 0.0021(5) 0.0057(5) P1 0.0233(5) 0.0211(5) 0.0207(5) -0.0017(4) -0.0001(4) 0.0002(4) P2 0.0239(5) 0.0225(5) 0.0180(5) -0.0004(4) 0.0007(4) -0.0040(4) O1 0.0250(14) 0.0277(15) 0.0209(14) 0.0022(12) 0.0035(11) -0.0018(12) O2 0.0222(13) 0.0242(14) 0.0210(14) 0.0018(11) 0.0015(11) -0.0026(11) C1 0.0236(19) 0.0215(19) 0.0204(18) -0.0026(15) 0.0022(15) -0.0027(15) C2 0.0254(19) 0.027(2) 0.0225(19) 0.0031(16) -0.0043(15) -0.0031(17) C11 0.0212(18) 0.0224(19) 0.0182(17) 0.0003(15) -0.0011(14) 0.0012(15) C12 0.037(2) 0.023(2) 0.029(2) 0.0002(17) 0.0021(18) -0.0078(18) C13 0.038(2) 0.025(2) 0.036(2) -0.0056(19) 0.0018(19) -0.0067(19) C14 0.031(2) 0.040(3) 0.024(2) -0.0063(19) -0.0019(17) 0.005(2) C15 0.038(2) 0.041(3) 0.019(2) 0.0024(18) -0.0010(17) -0.006(2) C16 0.040(3) 0.030(2) 0.023(2) 0.0023(17) -0.0023(18) -0.0092(19) C21 0.0210(19) 0.025(2) 0.028(2) -0.0064(17) 0.0054(15) -0.0027(16) C22 0.058(3) 0.033(3) 0.039(3) -0.003(2) -0.010(2) 0.008(2) C23 0.068(4) 0.027(3) 0.063(4) -0.008(3) -0.005(3) 0.007(3) C24 0.053(3) 0.042(3) 0.058(4) -0.028(3) 0.010(3) -0.009(3) C25 0.078(4) 0.047(3) 0.031(3) -0.015(2) 0.012(3) -0.015(3) C26 0.061(3) 0.032(3) 0.027(2) -0.0048(19) 0.010(2) -0.009(2) C31 0.026(2) 0.022(2) 0.035(2) -0.0038(17) 0.0080(17) -0.0009(17) C32 0.041(3) 0.040(3) 0.042(3) -0.015(2) -0.003(2) 0.001(2) C33 0.066(4) 0.039(3) 0.056(4) -0.026(3) 0.014(3) -0.007(3) C34 0.074(4) 0.021(2) 0.069(4) -0.008(3) 0.035(3) 0.000(3) C35 0.063(4) 0.029(3) 0.058(4) 0.010(3) 0.027(3) 0.018(3) C36 0.046(3) 0.026(2) 0.036(3) 0.0042(19) 0.015(2) 0.007(2) C41 0.0193(18) 0.023(2) 0.0228(19) -0.0035(15) -0.0042(15) 0.0053(15) C42 0.025(2) 0.030(2) 0.031(2) -0.0048(18) 0.0025(17) 0.0044(17) C43 0.026(2) 0.033(2) 0.041(3) -0.003(2) -0.0038(19) -0.0018(19) C44 0.036(2) 0.031(2) 0.038(3) -0.008(2) -0.012(2) -0.001(2) C45 0.042(3) 0.024(2) 0.028(2) -0.0072(17) -0.0019(19) 0.0051(19) C46 0.026(2) 0.023(2) 0.025(2) -0.0020(16) 0.0018(16) 0.0057(16) C51 0.024(2) 0.035(2) 0.0181(18) 0.0001(17) 0.0010(15) -0.0074(17) C52 0.042(3) 0.031(2) 0.022(2) -0.0045(18) 0.0041(18) -0.009(2) C53 0.058(3) 0.035(3) 0.035(3) -0.011(2) 0.004(2) -0.013(2) C54 0.055(3) 0.054(3) 0.033(3) -0.012(2) 0.001(2) -0.027(3) C55 0.034(3) 0.073(4) 0.031(3) -0.010(3) -0.002(2) -0.018(3) C56 0.025(2) 0.049(3) 0.029(2) -0.008(2) 0.0016(17) -0.010(2) C61 0.0267(19) 0.0216(19) 0.0215(18) -0.0006(16) 0.0012(15) -0.0005(16) C62 0.029(2) 0.029(2) 0.026(2) -0.0027(17) 0.0002(17) 0.0003(18) C63 0.043(3) 0.030(2) 0.023(2) -0.0056(17) 0.0040(18) 0.006(2) C64 0.043(3) 0.038(3) 0.023(2) 0.0036(19) 0.0104(19) 0.010(2) C65 0.036(2) 0.033(2) 0.026(2) 0.0088(18) 0.0102(18) -0.003(2) C66 0.033(2) 0.024(2) 0.026(2) 0.0013(16) 0.0027(17) -0.0034(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb C21 2.163(4) . ? Pb C11 2.185(4) . ? Pb O1 2.443(3) . ? Pb O2 2.471(3) . ? Pb S3 2.7035(12) . ? Pb S1 2.7143(12) . ? S1 C1 1.707(4) . ? S2 C1 1.648(4) . ? S3 C2 1.705(4) . ? S4 C2 1.649(5) . ? P1 O1 1.504(3) . ? P1 C41 1.783(4) . ? P1 C31 1.789(4) . ? P1 C1 1.841(4) . ? P2 O2 1.505(3) . ? P2 C61 1.786(4) . ? P2 C51 1.791(4) . ? P2 C2 1.836(4) . ? C11 C12 1.379(6) . ? C11 C16 1.380(6) . ? C12 C13 1.390(6) . ? C13 C14 1.385(7) . ? C14 C15 1.381(7) . ? C15 C16 1.383(6) . ? C21 C22 1.376(7) . ? C21 C26 1.382(6) . ? C22 C23 1.386(7) . ? C23 C24 1.382(9) . ? C24 C25 1.360(9) . ? C25 C26 1.395(7) . ? C31 C36 1.389(7) . ? C31 C32 1.400(7) . ? C32 C33 1.392(7) . ? C33 C34 1.371(9) . ? C34 C35 1.361(9) . ? C35 C36 1.386(7) . ? C41 C42 1.401(6) . ? C41 C46 1.408(6) . ? C42 C43 1.386(6) . ? C43 C44 1.407(7) . ? C44 C45 1.371(7) . ? C45 C46 1.392(6) . ? C51 C52 1.390(7) . ? C51 C56 1.394(6) . ? C52 C53 1.396(6) . ? C53 C54 1.362(8) . ? C54 C55 1.373(8) . ? C55 C56 1.393(7) . ? C61 C62 1.398(6) . ? C61 C66 1.400(6) . ? C62 C63 1.390(6) . ? C63 C64 1.377(7) . ? C64 C65 1.382(7) . ? C65 C66 1.386(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Pb C11 151.31(16) . . ? C21 Pb O1 87.17(13) . . ? C11 Pb O1 83.29(12) . . ? C21 Pb O2 81.31(13) . . ? C11 Pb O2 86.01(12) . . ? O1 Pb O2 133.96(10) . . ? C21 Pb S3 102.36(12) . . ? C11 Pb S3 99.48(11) . . ? O1 Pb S3 149.56(7) . . ? O2 Pb S3 76.41(7) . . ? C21 Pb S1 98.08(12) . . ? C11 Pb S1 105.62(11) . . ? O1 Pb S1 75.78(7) . . ? O2 Pb S1 149.84(7) . . ? S3 Pb S1 74.29(3) . . ? C1 S1 Pb 107.22(14) . . ? C2 S3 Pb 106.81(15) . . ? O1 P1 C41 110.16(18) . . ? O1 P1 C31 110.47(19) . . ? C41 P1 C31 110.2(2) . . ? O1 P1 C1 111.38(18) . . ? C41 P1 C1 106.07(19) . . ? C31 P1 C1 108.5(2) . . ? O2 P2 C61 111.22(18) . . ? O2 P2 C51 110.85(19) . . ? C61 P2 C51 109.45(19) . . ? O2 P2 C2 111.41(18) . . ? C61 P2 C2 107.5(2) . . ? C51 P2 C2 106.18(19) . . ? P1 O1 Pb 125.53(16) . . ? P2 O2 Pb 124.39(16) . . ? S2 C1 S1 125.6(3) . . ? S2 C1 P1 117.4(2) . . ? S1 C1 P1 116.9(2) . . ? S4 C2 S3 124.0(3) . . ? S4 C2 P2 118.5(2) . . ? S3 C2 P2 117.3(2) . . ? C12 C11 C16 121.6(4) . . ? C12 C11 Pb 119.2(3) . . ? C16 C11 Pb 119.2(3) . . ? C11 C12 C13 118.9(4) . . ? C14 C13 C12 120.0(4) . . ? C15 C14 C13 120.1(4) . . ? C14 C15 C16 120.4(4) . . ? C11 C16 C15 119.0(4) . . ? C22 C21 C26 120.1(4) . . ? C22 C21 Pb 120.9(3) . . ? C26 C21 Pb 118.9(3) . . ? C21 C22 C23 120.0(5) . . ? C24 C23 C22 119.7(5) . . ? C25 C24 C23 120.4(5) . . ? C24 C25 C26 120.3(5) . . ? C21 C26 C25 119.4(5) . . ? C36 C31 C32 120.0(4) . . ? C36 C31 P1 120.0(4) . . ? C32 C31 P1 119.2(4) . . ? C33 C32 C31 118.7(5) . . ? C34 C33 C32 120.6(6) . . ? C35 C34 C33 120.7(5) . . ? C34 C35 C36 120.3(6) . . ? C35 C36 C31 119.7(5) . . ? C42 C41 C46 119.5(4) . . ? C42 C41 P1 123.8(3) . . ? C46 C41 P1 116.7(3) . . ? C43 C42 C41 120.7(4) . . ? C42 C43 C44 118.8(4) . . ? C45 C44 C43 121.2(4) . . ? C44 C45 C46 120.3(4) . . ? C45 C46 C41 119.5(4) . . ? C52 C51 C56 119.7(4) . . ? C52 C51 P2 117.7(3) . . ? C56 C51 P2 122.6(4) . . ? C51 C52 C53 119.5(5) . . ? C54 C53 C52 120.2(5) . . ? C53 C54 C55 121.1(5) . . ? C54 C55 C56 119.8(5) . . ? C55 C56 C51 119.7(5) . . ? C62 C61 C66 119.4(4) . . ? C62 C61 P2 118.6(3) . . ? C66 C61 P2 121.4(3) . . ? C63 C62 C61 119.8(4) . . ? C64 C63 C62 120.2(4) . . ? C63 C64 C65 120.5(4) . . ? C64 C65 C66 120.2(4) . . ? C65 C66 C61 119.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Pb S1 C1 -70.01(18) . . . . ? C11 Pb S1 C1 93.67(18) . . . . ? O1 Pb S1 C1 14.97(16) . . . . ? O2 Pb S1 C1 -156.61(19) . . . . ? S3 Pb S1 C1 -170.65(15) . . . . ? C21 Pb S3 C2 91.38(19) . . . . ? C11 Pb S3 C2 -69.89(19) . . . . ? O1 Pb S3 C2 -162.8(2) . . . . ? O2 Pb S3 C2 13.62(17) . . . . ? S1 Pb S3 C2 -173.58(16) . . . . ? C41 P1 O1 Pb 122.6(2) . . . . ? C31 P1 O1 Pb -115.4(2) . . . . ? C1 P1 O1 Pb 5.2(3) . . . . ? C21 Pb O1 P1 87.1(2) . . . . ? C11 Pb O1 P1 -120.0(2) . . . . ? O2 Pb O1 P1 162.17(17) . . . . ? S3 Pb O1 P1 -22.7(3) . . . . ? S1 Pb O1 P1 -11.97(18) . . . . ? C61 P2 O2 Pb -124.8(2) . . . . ? C51 P2 O2 Pb 113.2(2) . . . . ? C2 P2 O2 Pb -4.8(3) . . . . ? C21 Pb O2 P2 -110.1(2) . . . . ? C11 Pb O2 P2 95.7(2) . . . . ? O1 Pb O2 P2 172.44(15) . . . . ? S3 Pb O2 P2 -5.03(17) . . . . ? S1 Pb O2 P2 -18.9(3) . . . . ? Pb S1 C1 S2 165.7(2) . . . . ? Pb S1 C1 P1 -18.1(3) . . . . ? O1 P1 C1 S2 -172.9(2) . . . . ? C41 P1 C1 S2 67.2(3) . . . . ? C31 P1 C1 S2 -51.2(3) . . . . ? O1 P1 C1 S1 10.5(3) . . . . ? C41 P1 C1 S1 -109.4(2) . . . . ? C31 P1 C1 S1 132.3(2) . . . . ? Pb S3 C2 S4 164.2(2) . . . . ? Pb S3 C2 P2 -21.0(3) . . . . ? O2 P2 C2 S4 -166.4(2) . . . . ? C61 P2 C2 S4 -44.3(3) . . . . ? C51 P2 C2 S4 72.8(3) . . . . ? O2 P2 C2 S3 18.5(3) . . . . ? C61 P2 C2 S3 140.6(2) . . . . ? C51 P2 C2 S3 -102.3(3) . . . . ? C21 Pb C11 C12 147.5(3) . . . . ? O1 Pb C11 C12 76.1(3) . . . . ? O2 Pb C11 C12 -148.8(3) . . . . ? S3 Pb C11 C12 -73.3(3) . . . . ? S1 Pb C11 C12 2.9(3) . . . . ? C21 Pb C11 C16 -30.7(5) . . . . ? O1 Pb C11 C16 -102.1(3) . . . . ? O2 Pb C11 C16 33.0(3) . . . . ? S3 Pb C11 C16 108.5(3) . . . . ? S1 Pb C11 C16 -175.3(3) . . . . ? C16 C11 C12 C13 -0.8(7) . . . . ? Pb C11 C12 C13 -179.0(3) . . . . ? C11 C12 C13 C14 0.8(7) . . . . ? C12 C13 C14 C15 -0.5(7) . . . . ? C13 C14 C15 C16 0.2(7) . . . . ? C12 C11 C16 C15 0.5(7) . . . . ? Pb C11 C16 C15 178.7(3) . . . . ? C14 C15 C16 C11 -0.2(7) . . . . ? C11 Pb C21 C22 -7.2(6) . . . . ? O1 Pb C21 C22 63.3(4) . . . . ? O2 Pb C21 C22 -72.0(4) . . . . ? S3 Pb C21 C22 -145.9(4) . . . . ? S1 Pb C21 C22 138.5(4) . . . . ? C11 Pb C21 C26 168.5(3) . . . . ? O1 Pb C21 C26 -121.1(4) . . . . ? O2 Pb C21 C26 103.7(4) . . . . ? S3 Pb C21 C26 29.7(4) . . . . ? S1 Pb C21 C26 -45.9(4) . . . . ? C26 C21 C22 C23 2.3(8) . . . . ? Pb C21 C22 C23 177.9(4) . . . . ? C21 C22 C23 C24 -1.0(9) . . . . ? C22 C23 C24 C25 -1.0(10) . . . . ? C23 C24 C25 C26 1.6(10) . . . . ? C22 C21 C26 C25 -1.6(8) . . . . ? Pb C21 C26 C25 -177.3(4) . . . . ? C24 C25 C26 C21 -0.3(9) . . . . ? O1 P1 C31 C36 -86.3(4) . . . . ? C41 P1 C31 C36 35.7(4) . . . . ? C1 P1 C31 C36 151.4(4) . . . . ? O1 P1 C31 C32 82.8(4) . . . . ? C41 P1 C31 C32 -155.2(4) . . . . ? C1 P1 C31 C32 -39.5(4) . . . . ? C36 C31 C32 C33 0.1(8) . . . . ? P1 C31 C32 C33 -169.0(4) . . . . ? C31 C32 C33 C34 0.0(9) . . . . ? C32 C33 C34 C35 -0.8(10) . . . . ? C33 C34 C35 C36 1.5(9) . . . . ? C34 C35 C36 C31 -1.4(8) . . . . ? C32 C31 C36 C35 0.6(7) . . . . ? P1 C31 C36 C35 169.6(4) . . . . ? O1 P1 C41 C42 173.9(3) . . . . ? C31 P1 C41 C42 51.8(4) . . . . ? C1 P1 C41 C42 -65.4(4) . . . . ? O1 P1 C41 C46 -7.4(4) . . . . ? C31 P1 C41 C46 -129.5(3) . . . . ? C1 P1 C41 C46 113.3(3) . . . . ? C46 C41 C42 C43 0.4(6) . . . . ? P1 C41 C42 C43 179.0(4) . . . . ? C41 C42 C43 C44 -0.4(7) . . . . ? C42 C43 C44 C45 0.3(7) . . . . ? C43 C44 C45 C46 -0.4(7) . . . . ? C44 C45 C46 C41 0.4(7) . . . . ? C42 C41 C46 C45 -0.4(6) . . . . ? P1 C41 C46 C45 -179.1(3) . . . . ? O2 P2 C51 C52 -4.2(4) . . . . ? C61 P2 C51 C52 -127.2(3) . . . . ? C2 P2 C51 C52 117.0(4) . . . . ? O2 P2 C51 C56 177.3(4) . . . . ? C61 P2 C51 C56 54.3(4) . . . . ? C2 P2 C51 C56 -61.5(4) . . . . ? C56 C51 C52 C53 -1.3(7) . . . . ? P2 C51 C52 C53 -179.9(4) . . . . ? C51 C52 C53 C54 0.6(8) . . . . ? C52 C53 C54 C55 -0.1(8) . . . . ? C53 C54 C55 C56 0.3(9) . . . . ? C54 C55 C56 C51 -1.1(8) . . . . ? C52 C51 C56 C55 1.6(7) . . . . ? P2 C51 C56 C55 -180.0(4) . . . . ? O2 P2 C61 C62 70.6(4) . . . . ? C51 P2 C61 C62 -166.6(3) . . . . ? C2 P2 C61 C62 -51.6(4) . . . . ? O2 P2 C61 C66 -100.7(4) . . . . ? C51 P2 C61 C66 22.2(4) . . . . ? C2 P2 C61 C66 137.1(4) . . . . ? C66 C61 C62 C63 -0.1(6) . . . . ? P2 C61 C62 C63 -171.5(3) . . . . ? C61 C62 C63 C64 0.2(7) . . . . ? C62 C63 C64 C65 -0.4(7) . . . . ? C63 C64 C65 C66 0.6(7) . . . . ? C64 C65 C66 C61 -0.5(7) . . . . ? C62 C61 C66 C65 0.3(6) . . . . ? P2 C61 C66 C65 171.5(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.883 _refine_diff_density_min -2.061 _refine_diff_density_rms 0.147 ### END data_2A1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H20 Cl O P Pb S2' _chemical_formula_weight 674.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.911(3) _cell_length_b 8.2427(17) _cell_length_c 20.384(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.468(16) _cell_angle_gamma 90.00 _cell_volume 2436.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 19.48 _cell_measurement_theta_max 21.06 _exptl_crystal_description needle _exptl_crystal_colour violet _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 7.286 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.534 _exptl_absorpt_correction_T_max 0.719 _exptl_absorpt_process_details 'ABSORB (DeTitta, 1985)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method omega-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 seconds' _diffrn_standards_decay_% 3.4 _diffrn_reflns_number 12040 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.98 _reflns_number_total 5309 _reflns_number_gt 4066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS CAD4' _computing_cell_refinement 'NONIUS CAD4' _computing_data_reduction 'DREADD (Blessing, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5309 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0391 _refine_ls_wR_factor_gt 0.0374 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb Pb 0.473132(7) 0.00516(2) 0.106577(6) 0.01564(4) Uani 1 1 d . . . Cl Cl 0.54558(6) -0.19347(11) 0.03293(4) 0.02114(18) Uani 1 1 d . . . P P 0.45338(5) -0.00451(14) 0.27539(4) 0.01521(15) Uani 1 1 d . . . S1 S 0.51957(6) -0.24880(11) 0.18656(4) 0.01880(18) Uani 1 1 d . . . S2 S 0.49949(6) -0.34433(12) 0.32247(5) 0.0244(2) Uani 1 1 d . . . O O 0.43938(14) 0.0936(3) 0.21151(10) 0.0180(5) Uani 1 1 d . . . C1 C 0.4917(2) -0.2110(4) 0.26152(16) 0.0175(7) Uani 1 1 d . . . C11 C 0.3263(2) -0.0330(4) 0.06390(15) 0.0154(8) Uani 1 1 d . . . C12 C 0.2623(2) 0.0333(4) 0.09651(16) 0.0202(8) Uani 1 1 d . . . H12 H 0.2820 0.0974 0.1360 0.024 Uiso 1 1 calc R . . C13 C 0.1693(2) 0.0036(6) 0.06992(16) 0.0268(7) Uani 1 1 d . . . H13 H 0.1245 0.0477 0.0913 0.032 Uiso 1 1 calc R . . C14 C 0.1415(2) -0.0900(5) 0.01249(18) 0.0273(9) Uani 1 1 d . . . H14 H 0.0777 -0.1110 -0.0050 0.033 Uiso 1 1 calc R . . C15 C 0.2053(2) -0.1529(5) -0.01957(17) 0.0235(8) Uani 1 1 d . . . H15 H 0.1856 -0.2158 -0.0594 0.028 Uiso 1 1 calc R . . C16 C 0.2988(2) -0.1243(4) 0.00627(16) 0.0202(8) Uani 1 1 d . . . H16 H 0.3432 -0.1675 -0.0156 0.024 Uiso 1 1 calc R . . C21 C 0.5908(2) 0.1672(4) 0.13554(16) 0.0176(7) Uani 1 1 d . . . C22 C 0.5851(2) 0.3286(4) 0.11867(17) 0.0212(8) Uani 1 1 d . . . H22 H 0.5289 0.3734 0.0934 0.025 Uiso 1 1 calc R . . C23 C 0.6629(2) 0.4255(5) 0.13920(18) 0.0271(9) Uani 1 1 d . . . H23 H 0.6598 0.5375 0.1279 0.033 Uiso 1 1 calc R . . C24 C 0.7438(3) 0.3609(5) 0.17553(18) 0.0287(9) Uani 1 1 d . . . H24 H 0.7968 0.4278 0.1889 0.034 Uiso 1 1 calc R . . C25 C 0.7488(2) 0.1974(5) 0.19290(17) 0.0272(9) Uani 1 1 d . . . H25 H 0.8048 0.1534 0.2187 0.033 Uiso 1 1 calc R . . C26 C 0.6724(2) 0.0990(4) 0.17270(16) 0.0206(8) Uani 1 1 d . . . H26 H 0.6754 -0.0130 0.1839 0.025 Uiso 1 1 calc R . . C31 C 0.3472(2) -0.0232(4) 0.30252(15) 0.0169(7) Uani 1 1 d . . . C32 C 0.2764(2) -0.1104(5) 0.26095(19) 0.0241(8) Uani 1 1 d . . . H32 H 0.2878 -0.1700 0.2238 0.029 Uiso 1 1 calc R . . C33 C 0.1899(2) -0.1098(5) 0.27373(19) 0.0265(9) Uani 1 1 d . . . H33 H 0.1410 -0.1670 0.2447 0.032 Uiso 1 1 calc R . . C34 C 0.1738(2) -0.0263(5) 0.32880(19) 0.0300(10) Uani 1 1 d . . . H34 H 0.1142 -0.0284 0.3380 0.036 Uiso 1 1 calc R . . C35 C 0.2436(3) 0.0596(5) 0.37019(19) 0.0304(10) Uani 1 1 d . . . H35 H 0.2321 0.1167 0.4079 0.037 Uiso 1 1 calc R . . C36 C 0.3307(2) 0.0631(5) 0.35699(17) 0.0243(8) Uani 1 1 d . . . H36 H 0.3788 0.1241 0.3850 0.029 Uiso 1 1 calc R . . C41 C 0.5411(2) 0.0843(4) 0.34092(17) 0.0187(7) Uani 1 1 d . . . C42 C 0.5896(2) 0.2154(4) 0.32359(18) 0.0232(8) Uani 1 1 d . . . H42 H 0.5738 0.2585 0.2792 0.028 Uiso 1 1 calc R . . C43 C 0.6611(3) 0.2825(5) 0.37172(19) 0.0319(9) Uani 1 1 d . . . H43 H 0.6942 0.3725 0.3602 0.038 Uiso 1 1 calc R . . C44 C 0.6845(3) 0.2197(5) 0.4364(2) 0.0348(10) Uani 1 1 d . . . H44 H 0.7353 0.2636 0.4685 0.042 Uiso 1 1 calc R . . C45 C 0.6349(3) 0.0946(5) 0.45425(19) 0.0351(10) Uani 1 1 d . . . H45 H 0.6496 0.0552 0.4993 0.042 Uiso 1 1 calc R . . C46 C 0.5634(2) 0.0251(5) 0.40700(16) 0.0249(8) Uani 1 1 d . . . H46 H 0.5295 -0.0626 0.4194 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb 0.01351(5) 0.02039(6) 0.01265(5) -0.00057(8) 0.00227(4) -0.00152(8) Cl 0.0227(4) 0.0247(5) 0.0165(4) -0.0008(4) 0.0054(3) 0.0036(4) P 0.0163(4) 0.0167(4) 0.0126(3) -0.0015(5) 0.0032(3) 0.0004(5) S1 0.0204(4) 0.0185(5) 0.0179(4) -0.0011(4) 0.0052(3) 0.0024(4) S2 0.0294(5) 0.0216(5) 0.0228(5) 0.0061(4) 0.0071(4) 0.0020(4) O 0.0205(12) 0.0196(14) 0.0142(12) -0.0001(10) 0.0049(10) 0.0023(10) C1 0.0125(16) 0.0201(19) 0.0185(17) -0.0007(15) 0.0012(13) -0.0016(14) C11 0.0146(15) 0.014(2) 0.0154(15) 0.0047(13) -0.0002(12) 0.0015(13) C12 0.0221(17) 0.020(2) 0.0163(16) -0.0018(14) 0.0004(13) -0.0007(15) C13 0.0185(15) 0.038(2) 0.0251(17) 0.002(2) 0.0076(13) 0.005(2) C14 0.0157(18) 0.037(2) 0.027(2) 0.0036(18) -0.0003(15) -0.0034(17) C15 0.0229(18) 0.027(2) 0.0181(18) -0.0013(16) 0.0007(15) -0.0059(17) C16 0.0211(18) 0.025(2) 0.0148(17) 0.0008(15) 0.0049(14) -0.0002(16) C21 0.0165(17) 0.024(2) 0.0142(17) -0.0035(15) 0.0070(13) -0.0045(15) C22 0.0185(18) 0.024(2) 0.0233(19) -0.0036(16) 0.0094(15) 0.0030(16) C23 0.032(2) 0.020(2) 0.034(2) -0.0082(17) 0.0152(18) -0.0048(17) C24 0.025(2) 0.032(2) 0.030(2) -0.0113(18) 0.0077(16) -0.0096(18) C25 0.0186(18) 0.041(3) 0.0196(19) 0.0009(18) -0.0008(15) -0.0008(18) C26 0.0209(18) 0.021(2) 0.0188(18) 0.0021(15) 0.0016(14) -0.0035(15) C31 0.0186(15) 0.018(2) 0.0148(15) 0.0048(15) 0.0046(12) 0.0048(15) C32 0.025(2) 0.020(2) 0.029(2) 0.0003(16) 0.0092(16) -0.0028(16) C33 0.0218(19) 0.017(2) 0.040(2) 0.0043(17) 0.0058(17) -0.0016(16) C34 0.0288(19) 0.025(3) 0.043(2) 0.0123(19) 0.0210(17) 0.0086(18) C35 0.039(2) 0.034(2) 0.023(2) 0.0037(17) 0.0172(18) 0.0138(19) C36 0.0250(19) 0.031(2) 0.0174(18) 0.0001(16) 0.0058(15) 0.0055(16) C41 0.0183(17) 0.0195(19) 0.0169(17) -0.0034(15) 0.0017(14) 0.0032(15) C42 0.029(2) 0.018(2) 0.0220(19) -0.0051(16) 0.0060(15) 0.0014(16) C43 0.033(2) 0.023(2) 0.039(2) -0.0084(19) 0.0087(18) -0.0090(18) C44 0.030(2) 0.032(2) 0.034(2) -0.015(2) -0.0076(18) -0.0014(19) C45 0.041(2) 0.036(3) 0.019(2) -0.0056(19) -0.0105(17) 0.005(2) C46 0.0282(17) 0.023(2) 0.0210(17) 0.0032(16) 0.0006(14) 0.0015(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb C21 2.175(3) . ? Pb C11 2.183(3) . ? Pb O 2.421(2) . ? Pb Cl 2.6186(9) . ? Pb S1 2.6445(10) . ? P O 1.505(2) . ? P C41 1.794(3) . ? P C31 1.802(3) . ? P C1 1.838(4) . ? S1 C1 1.703(3) . ? S2 C1 1.642(3) . ? C11 C16 1.375(4) . ? C11 C12 1.394(4) . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 C14 1.382(5) . ? C13 H13 0.9500 . ? C14 C15 1.376(5) . ? C14 H14 0.9500 . ? C15 C16 1.390(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C22 1.372(5) . ? C21 C26 1.393(5) . ? C22 C23 1.390(5) . ? C22 H22 0.9500 . ? C23 C24 1.369(5) . ? C23 H23 0.9500 . ? C24 C25 1.391(6) . ? C24 H24 0.9500 . ? C25 C26 1.381(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C36 1.388(5) . ? C31 C32 1.389(5) . ? C32 C33 1.375(5) . ? C32 H32 0.9500 . ? C33 C34 1.385(5) . ? C33 H33 0.9500 . ? C34 C35 1.374(5) . ? C34 H34 0.9500 . ? C35 C36 1.388(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C42 1.391(5) . ? C41 C46 1.398(4) . ? C42 C43 1.385(5) . ? C42 H42 0.9500 . ? C43 C44 1.383(5) . ? C43 H43 0.9500 . ? C44 C45 1.367(6) . ? C44 H44 0.9500 . ? C45 C46 1.383(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Pb C11 150.22(13) . . ? C21 Pb O 84.02(10) . . ? C11 Pb O 89.98(10) . . ? C21 Pb Cl 97.19(9) . . ? C11 Pb Cl 101.02(9) . . ? O Pb Cl 153.28(6) . . ? C21 Pb S1 103.88(9) . . ? C11 Pb S1 103.06(8) . . ? O Pb S1 76.83(6) . . ? Cl Pb S1 76.99(3) . . ? O P C41 110.80(16) . . ? O P C31 110.90(14) . . ? C41 P C31 110.31(15) . . ? O P C1 110.48(14) . . ? C41 P C1 107.06(15) . . ? C31 P C1 107.15(16) . . ? C1 S1 Pb 108.95(12) . . ? P O Pb 125.94(14) . . ? S2 C1 S1 124.6(2) . . ? S2 C1 P 118.24(19) . . ? S1 C1 P 117.19(19) . . ? C16 C11 C12 121.4(3) . . ? C16 C11 Pb 119.4(2) . . ? C12 C11 Pb 119.2(2) . . ? C13 C12 C11 118.5(3) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C14 C13 C12 120.3(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.0(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 119.3(3) . . ? C11 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C22 C21 C26 121.5(3) . . ? C22 C21 Pb 121.9(3) . . ? C26 C21 Pb 116.5(3) . . ? C21 C22 C23 118.9(3) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 120.6(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.1(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.2(3) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C21 118.7(3) . . ? C25 C26 H26 120.7 . . ? C21 C26 H26 120.7 . . ? C36 C31 C32 120.2(3) . . ? C36 C31 P 122.2(3) . . ? C32 C31 P 117.0(3) . . ? C33 C32 C31 119.7(3) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.2(4) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 120.3(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.1(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 119.5(3) . . ? C35 C36 H36 120.3 . . ? C31 C36 H36 120.3 . . ? C42 C41 C46 119.7(3) . . ? C42 C41 P 117.4(3) . . ? C46 C41 P 122.9(3) . . ? C43 C42 C41 119.4(3) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C44 C43 C42 120.5(4) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C45 C44 C43 120.3(4) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.3(4) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 119.9(4) . . ? C45 C46 H46 120.1 . . ? C41 C46 H46 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Pb S1 C1 84.76(15) . . . . ? C11 Pb S1 C1 -82.44(15) . . . . ? O Pb S1 C1 4.44(13) . . . . ? Cl Pb S1 C1 179.07(12) . . . . ? C41 P O Pb 113.91(17) . . . . ? C31 P O Pb -123.23(16) . . . . ? C1 P O Pb -4.6(2) . . . . ? C21 Pb O P -105.54(17) . . . . ? C11 Pb O P 103.68(16) . . . . ? Cl Pb O P -11.4(2) . . . . ? S1 Pb O P 0.26(13) . . . . ? Pb S1 C1 S2 173.56(17) . . . . ? Pb S1 C1 P -8.2(2) . . . . ? O P C1 S2 -173.06(17) . . . . ? C41 P C1 S2 66.2(2) . . . . ? C31 P C1 S2 -52.1(2) . . . . ? O P C1 S1 8.6(2) . . . . ? C41 P C1 S1 -112.2(2) . . . . ? C31 P C1 S1 129.50(19) . . . . ? C21 Pb C11 C16 118.0(3) . . . . ? O Pb C11 C16 -164.1(3) . . . . ? Cl Pb C11 C16 -8.6(3) . . . . ? S1 Pb C11 C16 -87.7(3) . . . . ? C21 Pb C11 C12 -63.2(4) . . . . ? O Pb C11 C12 14.6(3) . . . . ? Cl Pb C11 C12 170.1(2) . . . . ? S1 Pb C11 C12 91.1(3) . . . . ? C16 C11 C12 C13 0.8(5) . . . . ? Pb C11 C12 C13 -178.0(3) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C12 C13 C14 C15 -0.9(6) . . . . ? C13 C14 C15 C16 0.9(6) . . . . ? C12 C11 C16 C15 -0.8(5) . . . . ? Pb C11 C16 C15 177.9(3) . . . . ? C14 C15 C16 C11 0.0(5) . . . . ? C11 Pb C21 C22 -8.6(4) . . . . ? O Pb C21 C22 -88.0(3) . . . . ? Cl Pb C21 C22 118.8(3) . . . . ? S1 Pb C21 C22 -162.8(3) . . . . ? C11 Pb C21 C26 170.9(2) . . . . ? O Pb C21 C26 91.5(3) . . . . ? Cl Pb C21 C26 -61.7(3) . . . . ? S1 Pb C21 C26 16.6(3) . . . . ? C26 C21 C22 C23 0.1(5) . . . . ? Pb C21 C22 C23 179.6(2) . . . . ? C21 C22 C23 C24 0.1(5) . . . . ? C22 C23 C24 C25 -0.7(6) . . . . ? C23 C24 C25 C26 1.0(6) . . . . ? C24 C25 C26 C21 -0.7(5) . . . . ? C22 C21 C26 C25 0.2(5) . . . . ? Pb C21 C26 C25 -179.3(3) . . . . ? O P C31 C36 -105.5(3) . . . . ? C41 P C31 C36 17.6(4) . . . . ? C1 P C31 C36 133.8(3) . . . . ? O P C31 C32 65.6(3) . . . . ? C41 P C31 C32 -171.3(3) . . . . ? C1 P C31 C32 -55.1(3) . . . . ? C36 C31 C32 C33 0.4(5) . . . . ? P C31 C32 C33 -170.8(3) . . . . ? C31 C32 C33 C34 -1.7(6) . . . . ? C32 C33 C34 C35 1.5(6) . . . . ? C33 C34 C35 C36 0.0(6) . . . . ? C34 C35 C36 C31 -1.2(6) . . . . ? C32 C31 C36 C35 1.0(5) . . . . ? P C31 C36 C35 171.8(3) . . . . ? O P C41 C42 -6.4(3) . . . . ? C31 P C41 C42 -129.6(3) . . . . ? C1 P C41 C42 114.1(3) . . . . ? O P C41 C46 175.1(3) . . . . ? C31 P C41 C46 51.9(3) . . . . ? C1 P C41 C46 -64.4(3) . . . . ? C46 C41 C42 C43 1.8(5) . . . . ? P C41 C42 C43 -176.8(3) . . . . ? C41 C42 C43 C44 0.3(6) . . . . ? C42 C43 C44 C45 -2.7(6) . . . . ? C43 C44 C45 C46 2.8(6) . . . . ? C44 C45 C46 C41 -0.7(6) . . . . ? C42 C41 C46 C45 -1.6(5) . . . . ? P C41 C46 C45 176.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.793 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.105 ### END